AffA
              United Sr»t3j
              Env:,x>nrr»ntal Protection
              Agency
Of.'ice of Solid Waste
and Pmergency Resoonse
Washington. DC 20460
                                   £PA,530-SW-87
                                   OcTofier 1987 .
              Solid Want
Characterization  of MWC Ashes
and Leachates from MSW Landfills,
Monofills, and Co-Disposal Sites
               Volume V of VII
               Characterization of Municipal Waste
               Combustor Residues

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           FINAL  DRAFT
CHARACTERIZATION OF MUNICIPAL WASTE

         COMBUSTOR RESIDUES
           VOLUME V OF VII
               Versar, Inc
            6850 Versar Center
              P.O. Box 1549
          Springfield, Virginia 22151

                            /0

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            Contract No. 68-03-3235
              Delivery  Order  Mo.  3
               FINAL DRAFT  REPORT
         CHARACTERIZATION OF MUNICIPAL
            WASTE COMBUSTOR RESIDUES
                 Prepared for:

               Robert P. Hartley
     U.S. Environmental  Protection  Agency
Hazardous Waste Engineering Research Laboratory
            26 West St. Clair  Street
            Cincinnati, Ohio  45263
                 Prepared by:

                  Versar Inc.
               6850 Versar Center
                 P.O. Box 1549
         Springfield, Virginia  22151

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                             TABLE OF CONTENTS
 1.0  INTRODUCTION	 1-1

     1.1  Background	 1-2
     1.2  Objective	 1-4
     1.3  Summary of Approach	 1-5

 2.0  REVIEW OP PERTINENT LITERATURE	 2-1

 3.0  APPROACH TO STUDY	 3-1

     3.1  Municipal Waste Combustor Facility Selection	 3-1
          3.1.1  Facility Selection Criteria	 3-1
          3.1.2  Identification and Selection Process	 3-3
          3.1.3  Conformance to Selection Criteria	 3-4
     3.2  Facilities Selected	 3-2
          3.2.1  Facility A	 3-7
          3.2.2  Facility B	 3-10
          3.2.3  Facility C	 3-12
          3.2.4  Facility D	 3-15
          3.2.5  Summary of Facility Design and Operating
                 Characteristics	 3-17
     3.3  Samples and Sampling Procedures	 3-13
          3.3.1  Facility A	 3-21
          3.3.2  Facility B	 3-27
          3.3.3  Facility C	 3-34
          3.3.4  Facility D	 3-45
     3.4  Sample Preparation and Analysis Procedures	 3-52
          3.4.1  Laboratory Leachates	 3-53
          3.4.2  Analyses	 3-58

4.0  RESULTS AND DISCUSSION	 4-1

     4.1  Facility Operating Parameters	 4-1
     4.2  Solid Samples	 4-6
          4.2.1  Metals	 4-6
          4.2.2  Polychlorinated Biphenyls (PCBs)	 4-11
          4.2.3  Polychlorinated Dibenzo-p-dioxins and
                 Polychlorinated Dibenzo-furans (PCDD/PCDFs)	 4-17

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                             TABLE OF CONTENTS
                                (Continued)

     4.3  Laboratory Leachates	 4-29
          4.3.1  Metals	 4-29
          4.3.2  Polychlorinated Dibenzo-p-dioxins and
                 Pol/chlorinated Dibenzo-furans	 4-34
     4.4  Field Water Samples	 4-40
          4.4.1  Metals	 4-40
          4.4.2  Polychlorinatad Biphenyls	 4-44
          4.4.3  Polychlorinatad Dibenzo-p-dioxins and
                 Polychlorinated Dibenzo-Furans (PCDD/PCDFs)	 4-45
          4.4.4  Organic Constituents	 4-51
     4.5  Quality Assurance/Quality Control Summary	 4-56
          4.5.1  Internal QA/QC	 4-57
          4.5.2  External OA/QC	 4-80

5.0  EVALUATION	 5-1

     5.1  Comparative Evaluation With  Previously Reported
          Information	 5-1
          5.1.1  Solid Samples	 5-2
          5.1.2  Laboratory Leachates	 5-5
          5.1.3  Field Water Samples	 5-10
     5.2  Significant Trends in the  Data from this Study	 5-14
          5.2.1  Metals	 5-14
          5.2.2  Polychlorinated Biphenyls, Polychlorinated
                 Dibenzo-p-dioxins,  and Polychlorinated
                 Dibenzo-f urans	 5-19
     5.3  Relationships Between Facility Design and Operating
          Characteristics and Contaminant Concentrations	 5-22
          5.3.1  Metals	 5-23
          5.3.2  Polychlorinated Biphenyls, Polychlorinated
                 Dibenzo-p-dioxins,  and Polychlorinated
                 Dibenzo-f urans	 5-23
     5.4  Overall Assessment of Risk	 5-23
          5.4.1  Metals	 5-23
          5.4.2  Polychlorinated Biphenyls	 5-25
          5.4.3  Polychlorinated Dibenzo-p-dioxins	 5-25

6.0  CONCLUSIONS	 6-1

     APPENDIX A - References
     APPENDIX B - Analytical Methods for PCDD/PCDFs
     APPENDIX C - Analytical Methods for PCBs

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                               LIST OP TABLES
 Table 1.1     Samples  Collected From MWC Facilities	  1-7
 Table 1.2     Numbers  of  Analyses  Performed	   1-9

 Table 3.1     Facility Conformance to Selection Criteria	  3-5
 Table 3.2     Municipal Waste Combustor  Design and Operating
               Characteristics	  3-19
 Table 3.3     Landfill Characteristics	  3-20
 Table 3.4     Sample Identification Codes  for Facility A	  3-23
 Table 3.5     Sample Identification Codes  for Facility B	  3-29
 Table 3.6     Sample Identification Codes  for Facility C	  3-37
 Table 3.7     Sample Identification Codes  for Facility D	  3-46
 Table 3.8     Summary  Conditions for £P, TCLP, and MWEP Methods	  3-54
 Table 3.9     Summary  of  Analytical  Methods and Detection Limits	  3-59

 Table 4.1     Summary  of  Facility  A Operating Parameters	  4-2
 Table 4.2     Summary  of  Facility  B  Operating Parameters	  4-3
 Table 4.3     Summary  of  Facility  C  Operating Parameters	  4-4
 Table 4.4     Summary  of  Facility  0  Operating Parameters	  4-5
 Table 4.5     Total Metals Data for  Solid  Samples	  4-3
 Table 4.6     PCBs in  Solid Samples	  4-12
 Table 4.7     PCDD and PCDF in Solid Samples	  4-13
 Table 4.8     Extractable Metals Data  for  Three Laboratory
               Leaching Procedures	  4-31
 Table 4.9     PCDD and PCDF in Laboratory  Leachate Samples (TCLP)	  4-35
 Table  4.10     Extractable Organics Data for Three Leaching
               Procedures	  4-36
 Table  4.11     Total Metals Data for  Field  Water Samples	  4-41
 Table  4.12     PCBs in  Field Water Samples	  4-46
 Table  4.13     PCDD and PCDF in Field Water Samples	  4-48
 Table  4.14    Organic Constituents in  Field Water Samples	  4-52
 Table  4.15    QC Summary  (Internal)  for Metals	  4-58
 Table 4.16    QC Summary  (Internal)  for PCS Analysis	  4-63
 Table 4.17    QC Summary  (Internal)  for PCDD/PCDF Analysis	  4-69
Table 4.18    QC Summary  (Internal)  for Organic Analysis	  4-76
Table 4.19    QC Summary  (External)  for Metals	  4-81
Table 4.20    QC Summary  (External)  for PCS Analysis	  4-85
Table 4.21    QC Summary  (External)  for PCDD/PCDF Analysis	  4-88
Table 4.22    QC Summary  (External)  for Organic Analysis	  4-92

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                              LIST OF TABLES
                                (Continued)
Table 5.1     Comparative Evaluation of Total Metals in Solid
              Samples	 5-3
Table 5.2     Comparative Evaluation of PCBs in Solid Samples	 5-4
Table 5.3     Comparative Evaluation of PCDD/PCDFs in Solid
              Samples	 5-6
Table 5.4     Comparative Evaluation of Metals in EP Leachates	 5-8
Table 5.5     Comparative Evaluation of Metals in TCLP Leachates	 5-9
Table 5.6     Comparative Evaluation of Metals in Deionized
              Water Leachates	 5-11
Table 5.7     Comparative Evaluation of Total Metals in Field
              Water Samples	 5-12
Table 5.3     Comparative Evaluation of BNAs in Field Water
              Water Samples	 5-13
Table 5.9     Summary Results for Metals	 5-15
Table 5.10    Summary Results for PCBs, Dioxins, and Furans	 5-20
                              LIST OF  FIGURES
Figure 3.1    Facility A Combustor	 3-8
Figure 3.2    Facility B Combustor	 3-11
Figure 3.3    Facility C Combustor	 3-13
Figure 3.4    Facility D Combustor	 3-16

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                             ACKNOWLEDGEMENTS

      This  report was prepared by the staffs of Technical Operations and
 Laboratory Operations at Versar, Inc. and by Battelle, Columbus
 laboratory, Versar's subcontractor for analyses of municipal waste
 combustor  residues for polychlorinated dibenzo-dioxins and
 polychlorinated dibenzo-furans.  The contributions of the following
 individuals are gratefully acknowledged.
     Versar Inc.
     •     Dr. Wesley L. Bradford, Project Manager, Senior Hydrogeologist
     •     Mr. Arthur Jung, Task Manager, Senior Environmental Scientist
     •     Mr. David Basko, Environmental Engineer
     •     Ms. Pamela Hillis, Chemical Engineer
     Battelle, Columbus
     •     Dr. Fred DeRoos, Senior Analyst
     The assistance and guidance of Mr.  Robert P. Hartley during all
phases of this project is gratefully acknowledged.

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 1.0  INTRODUCTION
      This  report  is  the  final  deliverable  for Delivery Order Number  3  of
 Contract 68-03-3235.  The  report  (I)  describes the  planning, sampling  and
 analysis activities;  (2) summarizes the  results of  chemical analyses
 performed  on  fly  ash, bottom ash,  laboratory-prepared leachates  of fly
 ash and bottom ash,  field-collected quench water, leachate from
 mono-filled residue  landfills, and ground  water from monitoring  wells
 located near  the  landfills; and (3) evaluates the results of analyses
 with respect  to municipal  waste combustor  (MWC) facility design  and
 operation, variations among leachate  preparation procedures, and
 characterization of  the  residues as hazardous wastes.
      The remainder of this section discusses the background of this
 contract,  the objectives of the study conducted under Delivery Order
 No.  3,  and briefly summarizes the  technical approach taken in this study.
      Section 2 presents the results of a limited review of published
 literature characterizing MWC residues.
      Section 3 describes the approaches Versar took in selecting MWC
 facilities for sampling and analyses, describes the design and
 operational characteristics of the MWC facilities selected and their
 associated mono-filled landfills,   describes the sampling procedures  and
 samples collected at each MWC facility, and the sample handling  and
 analysis procedures.
     Section 4, presents and discusses the results of analyses of samples
 collected at the facilities by sample matrix (fly ash, bottom ash,
 laboratory-prepared leachate,  quench water, landfill leachate, ground
 water) and by major constituent category (heavy metals, polychlorinated
 biphenyls  (PCB's), polychlorinated dibenzo-dioxins and polychlorinated
 dibenzo-furans (PCDD/PCDP), and other organic constituents).
     Subsection 4.5 discusses  the   results of internal and external
quality assurance/quality control   (QA/QC) procedures exercised on the
analyses of the samples.
                                    1-1

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     In Section 5 the data obtained in this project is analyzed and
 evaluated in several respects.  In Subsection 5.1 the data is compared
 with selected data from the published literature and from other generally
 unpublished sources.  In Subsection 5.2 comparisons are made between the
 concentrations of constituents measured in laboratory-prepared leachates
 (Extraction Procedure, Toxicity Characteristic Leaching Procedure, and
 the Mono-filled Waste Extraction Procedure) and concentration of
 constituents measured in field-collected water samples (quench water,
 field leachate and ground water).   The objective of this comparative
 evaluation is to determine whether any of the extraction procedures
 currently required, or contemplated as being required in the future, for
 regulatory testing simulate actual environmental extraction processes.
 Subsection 5.3 provides a qualitative evaluation of the relationships
 observed in this study between MWC facility design and operating
 characteristics and the concentration of constituents observed in the
 residues.   Subsection 5.4 provides an overall assessment of the hazardous
waste characteristics of MWC residues.
     The conclusions of this study are summarized in Section 6.
     1.1  Background
     This  project was conducted under Delivery Order No. 3 of Contract
68-03-3235 administered through the U.S. EPA Hazardous Waste Engineering
Research Laboratory, Cincinnati, Ohio.  This contract was originally
entitled "Evaluation of Site Characteristics Contributing to Pollution at
Selected Hazardous Waste Disposal  Sites".
     Delivery Order No.  1 of this  contract dealt with the selection of a
 limited number of hazardous waste  disposal sites from several hundred
existing sites nationwide for in-depth study of site and contaminant
characteristics contributing to contaminant migration off-site.  Delivery
Order Mo.  1 was completed in July, 1985 with submittal of a final report
detailing the approach used in evaluating and selecting candidate sites
for in-depth investigation, and recommending five candidate sites, from
which one  would be selected.
                                    1-2

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      Delivery Order No.  2  involved five Tasks:   (I) establishing working
 relationships with the  selected  site owner/operator;  (2) preparing a
 detailed work plan for  investigations at  the site;  (3) acquiring existing
 site  information;  (4) conducting the investigation  as planned, and (5)
 reporting the results of the  investigation.  Delivery Order No. 2 was
 completed through  Task  3.  Tasks 4 and 5  were cancelled due to changing
 priorities within  the Agency  and to potential conflicts that the proposed
 investigation might cause with ongoing litigation at the candidate sites
 selected.
      Delivery Order No.  2 was amended in  February,  1986 creating a new
 Task  4 calling for an evaluation of the effectiveness of line/fly ash
 injection for stabilizing a typical solid waste  landfill.  Task 4 could
 not be completed because of unforeseen problems  gaining access to
 landfills both privately and publicly owned for  purposes of investigation.
 The results of the attempts to gain access to landfills were reported by
 letter in March and April, 1986.
      Delivery Order No. 3 of this contract, issued  in July, 1986, called
 for chemical  characterization of residues from municipal waste combustor
 facilities.   The title of the contract was changed  to "Characterization
 of Municipal  Waste Combustor Residues".   The performance and findings of
 the study conducted under this delivery order are reported herein.
     At the present time, the solid residues from MWC facilities are
 typically classified as non-hazardous and are placed in landfills
 regulated under Subtitle D of the Resource Conservation and Recovery Act
 (RCRA).
     Studies on the solid residues conducted in  the past few years,
however,  have shown the presence of heavy metals and organic compounds in
concentrations of potential concern.   Extraction Procedure (EP) Toxicity
Tests performed on fly ash samples have shown that  the concentrations of
some metals (primarily cadmium , chromium and lead) in the EP leachate
regularly exceed the  maximum concentrations for the hazardous waste
                                    1-3

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 characteristic of EP Toxicity.  In addition, polychlorinated dibenzo-
 dioxins  (PCDDs), polychlorinated dibenzo-furans  (PCDFs), and polychlorinated
 biphenyls  (PCBs) have been found in the fly ash  and flue gas from MWCs.
 PCDDs and  PCDFs have been reported in fly ash samples from MWCs in the
 United States, Canada, Europe, and Japan.
     The presence of some heavy metals in the EP leachate from fly ash at
 concentrations exceeding the regulatory limits, and the presence of
 potentially highly toxic organic compounds (PCDDs and PCDFs) in fly ash
 have raised questions concerning the proper disposal of MWC residues in
 general.  Of special concern is the issue of whether MWC residues
 disposal is adequately regulated under Subtitle D of RCRA.  In order to
 determine  (1) whether an alternative regulatory strategy is needed for
 MWC residues and (2) the structure of an alternative regulatory strategy,
 scientifically-defensible data chemically characterizing MWC residues are
 needed.
     The database presently available on chemical characterization,
however, is limited in size and scope (chemicals tested for).   Moreover,
the available data have generally been obtained using inconsistent
sampling techniques and analytical methodologies, and using uncertain or
inadequate quality assurance/quality control procedures.
     Work is underway under other EPA contracts to assemble information
on MWC residues from other sources (stata agencies, MWC facility '
operators,  etc.),  and initiatives have been submitted for chemical
characterization studies during Fiscal Years 1987 and 1988.  It is
expected that neither of these efforts will provide the scientifically-
defensible data needed for evaluation/development of alternative
regulatory strategies by the end of Fiscal Year 1937 when the Agency is
required to provide a preliminary report to Congress on this issue.
     1.2   Objective
     The objective of this project performed under this Delivery Order is
to collect chemical characterization data on residues from municipal waste
                                    1-4

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 combustor (MWC) facilities.   The residues characterized include fly ash
 from air emission control equipment,  bottom ash,  process quench water and
 leachate and/or ground water (when available)  from mono-filled landfills
 containing the solid residues.   In addition, ground water samples from
 any monitoring wells located near the landfills were to be characterized.
      This project is intended to provide  U.S.  EPA's Office of  Solid Waste
 with preliminary data characterizing  MWC  residues in advance of similar
 data to be provided in other studies  underway  or  scheduled for initiation
 in Fiscal Years 1987 and 1938.
      1.3  Summary of Approach
      This study was conducted in five Tasks briefly summarized below:
      Taste 1:   Preparation of Work Plan and Quality Assurance Project Plan
      The Work  Plan was  prepared  in accordance  with the  Scope of Work and
 in consultation with the  Project  Officer,  and  approved  August  15,  1986.
      Following approval of the Work Plan,  a Quality Assurance  Project
 Plan (QAPP) was  prepared  in  accordance with the guidance  for Category II
 projects and with "Interim Guidelines  and  Specifications  for Preparing
 Quality  Assurance  Project Plans"  (QAMS-005, December 29,  1980).   The QAPP
 was  approved with recommendations  on October 3, 1986.   During  the  course
 of  the study,  the  QAPP was revised to  respond  to  the recommendations made
 in conjuction  with the approval,  and to recommendations made pursuant  to
 a Technical Systems Audit and an Audit of  Data Quality  conducted at
 Versar on January  15, 1987.  The  final revised QAPP  was submitted
 February 3, 1987.
     Task 2;  Limited Literature Review
     A review of the published literature on the characterization  of MWC
 residues was conducted.  The scope of the  review was  limited to  an
 extension of more comprehensive reviews conducted previously and in
progress at the time of this study for the EPA Office of  Solid Waste.
                                    1-5

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 The  review was intended to (1) ensure that this study did not merely
 duplicate the MWC characterization work of others, (2) provide data for
 comparison with results of analyses obtained in this study, and (3) cover
 portions of the published literature which other studies may not have
 adequately examined.
     Task 3;  MWC Residue Sampling and Analysis
     This task was conducted in six (6) Subtasks as described below.
 EPA/HWERL assisted in identifying and assuring access to the MWC
 facilities at which samples were collected.
     Subtask 1 — Preliminary Survey of Facilities
     The lead technicians for each of two sampling teams with the
 supervision of the Project Manager and the Task Manager, made telephone
 contact with personnel at MWC facilities identified in order to
 (1) acquaint facility personnel with the objectives of the study,
 (2) determine general operating characteristics of the facilities (type
of combustor, characteristics of wastes accepted, combustor operating
conditions,  etc.), (3) determine locations for sampling solid residues,
field leachate and ground water, and (4) schedule dates for preliminary
site inspection and sampling.  These telephone interviews also
established whether the facility met the selection criteria as discussed
 in Section 3 of this report.
     Subtask 2 — Initial Site Visit and Inspection
     The lead technicians for each sampling team and the Task Manager
visited each of the four MWC facilities identified to obtain additional
detail on facility operation, locate points of access for collecting
residue samples,  identify locations for sampling field leachate and
ground water (if any), and establish working relationships with facility
personnel.
                                    1-6

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      Subtask 3  — Sample Collection
      Samples of MWC  solid residue, field laachate, and ground water were
 collected  at sampling points identified in Subtask 2 above.
      The lead technician and one addition sampling technician collected
 the  samples.  Procedures for sample collection, preservation,
 documentation,  and shipment to the laboratory are described in detail in
 Section 3  of this report.
      The number of samples of each medium actually collected are
 summarized in Table  1.1 below.

            TABLE 1.1  SAMPLES COLLECTED FROM MWC FACILITIES
                 Liquid Samples
Solid Samples

Facility
A
B
C
0
(^•) Samples
A
B
C
D
Field
Leachate
0.
3
3
3
include
—
	
	
1
Ground
Water
1
1
4
0
Quench
Water
2
3
2
3
Bottom
Ash
6
6
7
6
Fly
Ash
7
6
9(3)
7
Landfill
Composite


1
1
the following duplicates
	
	
- —
	
—
1
	
1
1
1
2
1
2
1
1
2
,. —
	
	
	
    Samples include one composite at each facility for preparation of
       laboratory leachates, plus 3 composite duplicates.
    Samples include grab samples of 3 different size fractions of
       fly ash.
     In addition, 4 trip blanks consisting of deionized water from the
Versar laboratory, carried to the facility, handled like a sample, and
returned for analysis were taken.  And 2 field blanks consisting of
deionized water poured over and through the cleaned sampling devices and
returned for analysis were collected.
                                    1-7

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     Subtaak 4 — Sampla Analyses
     Solid residue samples (fly ash and bottom ash)  and liquid samples
 (field leachate, ground water and quench water) and leachates prepared in
 the laboratory from the solid residue samples were analyzed for various
 heavy metals and organic compounds.  The laboratory leachates were
 prepared using the Extraction Procedure (EP), the Toxicity Characteristic
 Leaching Procedure (TCLP), and the Mono-fill Waste Extraction Procedure
 (as described in SW-924).   Sequential extractions were performed using
 the monofill waste extraction procedure.  Total Organic Carbon (TOC)
 analyses were performed on all field water samples (plus blanks) and on
 the laboratory leachates prepared by the SW-924.   Analyses for total
metals were performed on all field water samples, laboratory leachates,
and solid residue samples.
     An organic scan was performed on field water samples and laboratory
 leachates to determine whether organic compounds other than PCDDs, PCDFs,
and PCBs were present.  Selected field water samples and laboratory
 leachates were solvent extracted and the compounds present in each
fraction (acid and base/neutral) were identified and quantified by GC/MS
techniques (EPA Method 625).  The selection of the field water samples
and laboratory leachates for extraction and GC/MS analysis was based
 largely on the TOC concentrations.
     Analyses for PCDDs and PCDFs were performed by the Battelle, Columbus
 laboratory (Versar's subcontractor for these analyses) on all fly ash
samples and on selected bottom ash and field water samples.  In addition,
analyses were performed on TCLP leachates of 8 ash samples.  PCDD/PCDFs
were identified and quantified at the homolog level; the 2,3,7,3 tetra-
chlorodibenzo-dioxin isomer was quantified separately.
     Analyses for PCBs were performed on all solid residue and field water
 samples.  No PCS analyses were performed on laboratory leachates.  The
PCBs were identified and quantified at the homolog level rather than as
Arochlors.
                                    1-8

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     The numbers of analyses for each group of constituents in each

 medium actually performed  in this study are summarized in Table 1.2.
                 TABLE 1.2  NUMBERS OF ANALYSES PERFORMED
            (Including duplicates, trip blanks and field blanks)
Field Liquid
Analyses Samples
TOC
Metals (2)
Organic Scan
Organic Constituents
PCS
PCDD/PCDF(6)
31
29(3)
24(3)

27
22
Laboratory
Leachates
20<1)
48
44
32

8<7)
Solid
Residues

42


45
43
 (l>Total organic carbon (TOC) analyses not performed on laboratory
   leachates prepared by the EP and TCLP procedures because acetic acid
   is used for pH adjustment.

 (2>Total metals include copper, chromium, cadmium, lead, arsenic,
   selenium, mercury, iron, manganese, zinc, and nickel.

 (^Duplicates and field blanks, but not trip blanks.
       organic scan consists of extraction with Freon 113 and
   quantification of total organics using an infrared spectrophotometer.

(5>No duplicates performed on the organic scan.

(^Analyses performed by subcontractor (Battalia Columbus Laboratories).

<7>PCDD/PCDF analyses of TCLP leachates, one from each solid residue
   composite from each facility.


     Subtask 5 — Analytical Data Management

     The analytical data from the laboratory were entered into a computer

system (i.e.,  IBM-PC and Lotus 1-2-3 software) to generate data tables
                                    1-9

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 and graphs.  Field data, that is information describing the MWC facility
 design and operating conditions, were also entered into the data base.
 The data were arranged by MWC facility and variable or chemical
 constituent.  In cases where data comparisons would be meaningful (e.g.,
 to examine the differences between laboratory leachate and field water
 sample analyses), the data were grouped together or graphs were prepared
 thereby highlighting significant trends.  The compilation of all
 analytical data includes the presentation of all quality assurance/
 quality control data (e.g., results form the analysis of replicates,
 percent recoveries of spikes or surrogates).
     Subtask 6 — Ongoing QA Review
     The analytical and quality assurance/quality control procedures were
 detailed in the QAPP for this project.  Each of the analytical procedures
 (e.g., typically CLP methods) employed include quality control measures
 to evaluate the performance of the method on a continuing basis.  These
 performance criteria were evaluated as specified by the method by the
 laboratory and project QA/QC officer, and any deficiencies were resolved
 either through re-analysis of the sample or the application of
appropriate correction factors.   In addition, replicate analyses were
 performed on 25 percent of all samples tested.  The results of the
 replicate analyses, as well as the procedural performance checks (e.g.,
 spike or surrogate recoveries),  are presented in a separate section of
 this report so that the information may be interpreted in terms of the
actual level of confidence of the data.
     Task 4;   Data Evaluation
     As the analytical and quality control data became available, efforts
were directed toward reviewing the data and field notes and interpreting
the results.   Based on EPA's concern regarding the environmentally safe
disposal of MWC residues, the following technical concerns were addressed
during the evaluation of the data:
                                   1-10

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     1.   Recant data available in the literature  suggests  that  toxic
         constituents (e.g.,  metals,  organics)  may be  present  in solid
         waste residues generated by  MWC facilities.   The  data  derived
         from this study were used to further  examine  whether  a problem
         associated with the  land disposal  of  MWC residues exists.

     2.   The  results of the analyses  of  the field water  samples and
         laboratory leachates were compared to determine if any of  the
         laboratory leaching  procedures  accurately model the constituents
         found in  the field water samples.

     3.   At each MWC facility,  operating data  were collected to
         characterize the combustion  conditions which  resulted  in
         production of the residues that were  sampled.   The results of the
         chemical  analyses of solid and  liquid samples,  and laboratory
         leachates were examined  with respect  to  the combustion conditions
         to identify any significant  correlations.

     Task 5:   Project Report  and  Summary Report Preparation

     The project  report (including draft and  final) has been prepared by

the  Versar technical  specialists  who were  assigned as team leaders for

each facility  sampled.   Versar senior scientists  contributed to and

reviewed the  report  to ensure that the  overall project  objectives  are met

and  that the final  report is technically sound and complete.

     The report includes:

     •  Results of  the  literature  review.

     •  All analytical  results and field observations.

     •  All quality assurance and  quality control  and data.

     •  An interpretation of the significance of  the data  in light of
        current disposal practices for MWC wastes  and the  findings of
        other groups working on MWC  residues.

     A Project Summary will  be prepared, based on  the draft report, to be

published by EPA and included in the EPA/600 series of  Research and

Development Project Summaries.
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 2.0  REVIEW OF  PERTINENT LITERATURE
      Versar performed a limited literature review to obtain pertinent
 information from previous studies of municipal waste combustion  (MWC).
 This  review focused on acquiring literature that contained MWC residue
 characterization data.  This acquired data was then used for a
 comparative evaluation with the MWC residue characterization data
 generated in this study (see Section 5.1).
      The literature review was performed by using the following  sources:
 a database  of abstracts on MWC ash literature compiled by the University
 of  Massachusetts; the Dialog computer user service, which is a
 compilation of  technical document abstracts that are accessed by
 "keywords"  (e.g., fly ash, bottom ash, municipal waste combustion,
 leachate, etc.); and Versar's in-house technical documents.  These
 sources were used to obtain more than 250 abstracts from potentially
 pertinent documents.  Then, each of the abstracts was read to determine
 whether the publication contained information warranting its
 acquisition.  Because the focus of the literature review was MWC residue
 characterization data, the publications describing topics such as
 incinerator design, landfill design, analytical techniques for
 characterizing the residue, stock sampling and analysis, and residue
 utilization were omitted from any further consideration.
     After  the review of the abstracts was completed, 78 documents were
 identified as potential sources of MWC residue characterization  data were
 acquired.  The identified documents are listed in Appendix A.  Each of
 these documents was scanned to extract data for metals, polychlorinated
 biphenyls (PCBs),  polychlorinated dibenzo-p-dioxins/polychlorinated
 dibenzofurans (PCDD/PCDF), and organic constituents (i.e., base/neutral
 and acid extractable semi-volatile compounds-BNAs) in solid samples
 (e.g., fly ash and bottom ash), laboratory leachates prepared from these
 solid samples,  and field water samples (e.g., field leachate, quench
water, and ground water).   This scan of the publications revealed an
                                    2-1

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abundance of data for metals and PCDD/PCDF in solid samples,  indicating
that the metal and PCDO/PCDF composition of the solid MWC residues has
been extensively studied.  This information was extracted from the
publications and is summarized in Section 5.1 (see Tables 5.1 and 5.3).
A limited amount of data was also available for PC3s in solid samples;
metals in Extraction Procedure (EP), Toxicity Characteristic  Leaching
Procedure (TCLP), and deionized water laboratory-prepared leachates; and
metals and BNAs in field water samples, including quench water and field
leachate.  This information is also summarized in Section 5.1 (see
Tables 5.2,  5.4, 5.5, 5.6, 5.7, and 5.8).  Finally, the reviewed
publications did not contain any data for PCDD/PCDFa and BNAs in
laboratory-prepared leachates, or for PC3s and PCDD/PCDFs in field water
samples, indicating that the previous studies did not address these
contaminant/matrix combinations.
                                    2-2

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 3.0  APPROACH  TO  STUDY
      This  section discusses  in detail the approach employed  in this
 investigation.  Section  3.1  describes the process of selecting the four
 MWC facilities sampled including the selection criteria and  the
 identification and selection process.  Section 3.2 provides  a description
 of  each of the facilities selected including the design and  operating
 characteristics of the combustor units and pertinent characteristics of
 the  landfills  into which the MWC residues are disposed.  Section 3.3
 details the sampling procedures, sampling locations and samples collected
 at  each facility.  Section 3.4 describes the procedures used in the
 laboratory for preparing leachates, and the procedures for analyses of
 all  samples and laboratory-prepared leachates.
     3.1  Municipal Waste Combustor Facility Selection
     Four MWC facilities were selected for residue chemical
 characterization.  These facilities were chosen to (1) represent MWC
 facilities generally in design and operating features, (2) provide a
 range of design and operating features such that any difference observed
 in the chemical characteristics of the residues could possibly be
qualitatively related to design and operating features, and  (3) provide
samples of landfill leachate generated exclusively from MWC  residues
rather than from mixtures of MWC residues and other solid wastes.
     3.1.1  Facility Selection Criteria
     The four MWC facilities studies in this project were selected from a
larger group of facilities known to EPA/HWERL and EPA/OSW in accordance
with the following criteria:
     1.  Facility Types  - Two facilities were to have resource (e.g.,
         energy or material)  recovery processes,  and two were to be
         operated solely for waste volume reduction.
     2.  Information Availability - Each facility was to be currently
         active and was  to have information available on the engineering
         design,  operating characteristics  (e.g.,  times,  temperatures,
         refuse feedrate,  etc.),  raw waste  characterization  (e.g..
                                   3-1

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         amounts of industrial wastes accepted and approximate percentages
         of paper, food, plastic, textiles, etc.), and relative amounts
       .  and disposition of the various MWC residues (e.g., fly ash,
         bottom ash, quench water, etc.).

     3.  Landfill ing of Solid Residues - Each facility was to have
         disposed of the MWC residues in a cell or landfill separate from
         other solid or hazardous wastes.

     4.  Suitability of Sampling Locations - The MWC facility and the
         landfill should be designed to permit the collection of discrete
         samples of the individual residues (fly ash, bottom ash, quench
         water).

     5.  State and Facility Cooperation - To ensure that the sampling and
         information gathering efforts would be performed in an efficient
         and timely manner without obstructions due to any policy or
         regulatory enforcement issues, representatives of the cognizant
         state regulatory agency and of the facility should be willing to
         cooperate with EPA/HWERL and contractor personnel.

     Criteria 2, 3, and 5 were considered absolute, i.e., no facility

would be selected that did not meet these three criteria.  With respect

to Criterion 1, it was important that both resource recovery and volume

reduction facilities be studied, but the relative proportions of the two

types were flexible.  In fact, among the four MWC facilities selected,

three were energy recovery facilities (one with a material recovery

process proceeding combustion) and one was a volume reduction facility.

With respect to Criterion 4. optimally separate samples of fly ash and

bottom ash should be collected.  However, combined bottom and fly ash
samples were considered acceptable if a separate fly ash sample could be

collected and the approximate fraction of fly ash in the combined ash was

known.

     Other desirable features of the MWC facilities included the

following:

     •  The landfill containing the mono-filled MWC residues should have
        an operating leachate collection system from which samples of
        field leachate could be collected.  Alternatively, locations,
        where leachate could be obtained should be available.
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      •  Monitoring wells  from which ground water  samples  could be
         collected should  be  located down gradient in a  water-bearing zone
         potentially affected by leachate from the landfill.
      3.1.2   Identification and Selection Process
      EPA/HWERL and EPA/OSW first  identified the states  which currently
 require  that MWC  residues  be disposed of in a separate  cell  or landfill.
 This  assured that  any facility selected would have a monofill disposal
 area  rather than a landfill  with  co-disposed solid wastes and/or
 hazardous wastes.   EPA/HWERL subsequently contacted representatives  of
 the cognizant regulatory agencies within each state to  (1) enlist their
 cooperation in the  project/  and (2)  determine MWC facilities  that might
 meet  the selection  criteria.   Subsequently, letters were  sent to the
 state  regulatory agencies  describing the objectives of  the project,
 presenting a timetable for facility  selection and sample  collection,  and
 formally requesting the state  agency's assistance.
     The state agencies agreeing to  assist the project  then contacted the
 facilities to briefly describe  the project and to enlist  the  cooperation
 of facility representative.  Upon receipt of notification that facilities
 had been contacted and had agreed to cooperate in the project, letters
 were sent from EPA/HWERL to  the individual facilities describing the
 objectives of the project, and proposing a schedule for initial  telephone
 interviews,  site visits, and sample collection by Versar personnel.
     Once agreement had been reached of the facility's cooperation in  the
 project,  Versar personnel  contacted facility representatives  by  telephone
 and obtained specific detailed information on the combustor facility
 design and operating characteristics including the feed waste materials,
 ash handling system, residue disposal practices, characteristics  of  the -
 disposal  cell or landfill, and the availability of locations  for sample
collection.   A questionnaire was developed and used for guidance  in
conducting these telephone interviews.
                                    3-3

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     The information obtained in the telephone interviews was used to
make the final selection of the four facilities to be sampled.   Some
facilities initially considered were eliminated at this point.
     Subsequently, the Versar lead sampling technician and the  Task
Manager (or designee) visited the facility to determine exact sampling
locations and the working conditions to be encountered during sampling/
and to make final arrangements with facility personnel on sampling
schedule and any special assistance required during sampling.  The
information obtained in these initial site visits was used to plan the
sampling activities/ including the sampling equipment and sample
containers required/ and the sampling strategy (e.g. time compositing
versus spatial compositing).  The actual sampling was conducted within
three weeks of completion of the initial facility visits.  Sampling
locations and procedures are described in detail for each facility in
Section 3.3.
     3.1.3  Conformance to Selection Criteria
     The degree to which each facility selected met the criteria for
selection is summarized in Table 3.1.
     Among the four facilities, three were operated for energy recovery
with one (Facility A) having some limited capability for recovery of
aluminum from the feed prior to combustion.  One facility was operated
for volume reduction only.
     All four facilities provided detailed information on the combustor
design and operating characteristics and made available as much
information as they had on the design of the landfill receiving the solid
residues.   At all four facilities/ the solid residues were disposed in
monofill landfills.
     At three of the facilities/ bottom ash and fly ash were combined and
there was no feasible way to collect a separate bottom ash sample.  At
all facilities, however, separate fly ash samples were collected.
                                    3-4

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            TABLE  3.1    FACILITY  CONFORMANCE TO SELECTION CRITERIA
CRITERIA
i . Facility Types
2. Information Available
3. Monoflll Disposal
4. Sampling Locations
FACILITY
A
RR/ER
Yes
ves
Fly &
Combined
a
ER
Yes
Yes
Fly &
Bottom
c
VR
Yes
Yes
Fly &
Combined
D
ER
Yes
Yes
Fly &
Combined
5. State/Facility
     Cooperation
Yes
Yes
Yes
                                        Yes
Other:

 • Leacnate Collection System   No
 • Monitoring wells             1
               NO
               1
               NO
               4
             NO
             0
RR » Resource Recovery; aluminum recovery oefore combustion.
ER = Energy Recovery as steam.
VR a volume Reduction only.
                                   3-5

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    Although some of the landfills associated with the facilities had
leachate collection systems in place,  none were functioning as designed
at the time of sample collection for this scudy.   Samples of field
leachate were collected at three of the facility landfills (B, C, and D)
at locations of opportunity as described later.
     Suitably-placed monitoring wells  were available and were sampled at
three of the facilities (A, B, and C).
     Overall, the criteria for facility selection were achieved with
reasonable success in the four facilities selected.  The two main areas
of deficiency with respect to the criteria were in the access to fly ash
and bottom ash separately in the ash processing line and the lack of
functioning leachate collection systems at landfills.
     Further inquiry by Versar personnel has indicated that few combustor
designs provide access to fly ash and bottom ash separately.  In the
limited time available to conduct the  search for MWC facilities, it was
not possible to locate more than one such combustor.
     A leachate collection system, which was present at only one facility
had apparently become clogged and was  not draining.  This may be a
pervasive problem with mono-filled disposal cells containing MWC residues
which have been in operation for more  than a few years.
     3.2  Facilities Selected
     Based upon the selection criteria presented in Section 3.1.1 and the
involvement of EPA and appropriate state agencies, four facilities were
selected for MWC residue characterization sampling.  Because each of the
facilities was assured that the source of the data for this study would
not be identified, the facilities were generically designated throughout
this report as Facility A, B, C, and D.  After the facilities were
selected, they were contacted by telephone and visited prior to  sampling,
to obtain operating and design characteristics of  the incinerators and
                                    3-5

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 their associated landfills.  Sections 3.2.1 through 3.2.5 present descrip-
 tions and summary tables of these operating and design characteristics
 for each facility.
     3.2.1  Facility A
     Facility A operates two water-wall rotary combustors which were put
 on line in December 1981 and March 1982.  Figure 3.1 presents a diagram
 of a typical rotary combustor.  The units are each rated at 100 tons per
 day and operate 24 hours per day, 7 days per week.  The total actual
 operating capacity is about 150 to 180 tons per day, depending on the
 moisture content of the feed.  Each unit is equipped with a mechanical
 cyclone separator and an electrostatic precipitator.
     The units were originally the same, but Unit 2 has been retrofitted
 to provide better air control.  The majority of the air to Unit 1 is
 overfire.   Unit 2 was retrofitted to better control the percentage of
 overfire and underfire air.
     The units are monitored using televisions to maintain the fire in
 the middle of the combustor area.  In addition, oxygen, carbon monoxide,
 furnace temperature, and residues are monitored to determine the
 combustion efficiency.  The feed rate and the amount of combustion air
 are changed to control the combustion.
     The feed to the units is approximately 50 percent residential and
 50 percent industrial (i.e., construction type refuse including wood,
 plastic, and metal).  The facility has the ability to separate glass,
 iron,  and aluminum from the feed, but does not process all feed to the
 combustors.   From the refuse pit, the bucket feeds the two charging
hoppers (See Figure 3.1) to the combustors and the charging hopper to the
 separation process.   The processed feed is discharged back into the
 refuse pit,  where it is used to feed the combustor charging hoppers.
Occasionally,  the refuse in the pit covers the inlet or the outlet of the
separation process making it impossible to process refuse.  When refuse
                                    3-7

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                        Figure  3.1  Facility A Combustor
                                 BOIL2R
           ROTARY COMflUSTOR
1 Charging Hopp«r
2 Charging Raa
3 Trunnion for Sarrtl Rocacion
4 Wind Box and A»h Removal
3 Uaecr Cooling Sysetfl Kocary Joint
4 Final Burnout Zon*
7 Primary A»h Oischargt Chutt
8 Aih Qu«nch Tank
                                              CROSS-SECTION  OP
                                              ROTARY COMBUSTOR
                                       3-8

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 is  processed, the aluminum is recycled, but the glass and iron are
 disposed at the landfill along with the ash.
     The residues from the combustors include bottom ash, fly ash, and
 quench water.  The units achieve approximately 90 percent reduction by
 volume and 50 to 60 percent reduction by weight of -the incoming,  refuse.
 The bottom ash falls into a quench tank and is drag conveyed to  a
 temporary storage bin which has sufficient capacity to hold the  ash
 produced over 4 hours (i.e., 14 to 18 cubic yards).  The fly ash, which
 is removed from the flue gas using mechanical cyclone separators and
 electrostatic precipitators, enters a turbulator where water is  added.
 The fly ash feeds to the quench tank displacing some quench water.  The
 displaced quench water (i.e., approximately 10 to 15 gallons per minute
 total) overflows to a sump where solids are.removed  The effluent from
 the sump is discharged to the sanitary sewer.  The bottom and fly ash,
 along with non-combustible and large items (i.e., large metal items,
 tires, wood palettes, furniture, etc.), are transported to a landfill a
 total of about 12 times per day.
     The landfill is located about 13 miles northwest of the facility.
 It was used for municipal refuse until about early 1982 when the
 combustors came on line.   The landfill is now used for ash, separated
 glass and iron, and large items.  The ash has been segregated from the
 municipal refuse.   A small creek runs close to the landfill (i.e.,
 200 yards).   There is no leachate collection system, but there are two
 ground-water monitoring wells in the new section of the landfill where
 the ash is placed.   The landfill is surrounded by a berm that limits the
 release of surface runoff to adjacent areas.  One monitoring well that is
 closer to the older ash is reported to be frequently dry.  The second
monitoring well,  which contains water, is closer to the freshly  placed
 ash, but at  quite  a distance (i.e., 400 to 500 feet).  The landfill is
 covered daily with soil.
                                    3-9

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      3.2.2  Facility B
      Facility B operates three water-wall traveling grate mass burn
 combustors similar to the unit shown in Figure 3.2.  Units 2 and 3 were
 put on  line in 1974.  Unit 4 was put on line in September, 1986.  Units 2
 and 3 are each rated at 360 tons per day, and Unit 4 is rated at 400 tons
 per day.  The units operate 24 hours per day, 7 days per week.  The total
 actual  operating capacity is about 600 to 700 tons per day, but will be
 up to 900 tons per day when Unit 4 is completely operational.  The feed
 to the  units is approximately 30 percent residential and 20 percent
 commercial.  Combustion efficiency is controlled by changing the amount
 of underfire air to produce the required steam flow (i.e.,
 30,000  Ibs/hour each unit).  Each unit is equipped with a cyclone and an
 electrostatic precipitator for participate control.
     The residues include bottom ash, fly ash,  and quench water.  The
 units achieve approximately 90 percent reduction by volume and 70 percent
 reduction by weight of the incoming refuse.   The bottom ash is spray
 quenched (i.e.-,  approximately 20 to 25 gallons  per minute each unit),
 stored  in an enclosed hopper, and discharged into a disposal trailer (See
 Figure 3.2) about every two hours (i.e., 3 to 4 hoppers of bottom ash per
 combustor per shift).   Each trailer has sufficient capacity to hold two
 bottom ash dumps.   Fly ash from each unit is removed from the flue gas
 stream  in separate cyclones and electrostatic precipitators, mechanically
 conveyed (i.e.,  screw conveyors) to a combined duct,  and discharged to an
 enclosed storage bin through a large hose.   The quench water is discharged
from the bottom  ash hoppers,  spills to the pavement below, and is
collected in a surface drain.  The quench water is discharged to the
 sanitary sewer after solids are removed in a sump.
     The landfill  is located about five miles east of the facility and
has been used for the disposal of bottom ash and fly ash for about 4 to
 5 years.  The landfill was estimated to be approximately 15 acres
 (rectangular)  in surface area and about 40 feet deep.   The ash is
                                   3-10

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                        Figure  3.2  Facility B Combustor
                          INCINERATOR SIDE VIEW

                               HEATING PLANT
 I. C1ANI
 2. CHANGING NCWH
 3. SOUO WASTf COMPACTQI TtAIUI
 4. «3U« UVU tKlMOCATINO O*ArU
 i. SOUO WASTf STOIACI MT
 4. raiCfD OlAfT FAN
 7. ASH HOPPft
 I. ASH OIS^OSAI TIAIIH
 9. AUXIIIAIT IUINU
10. OUST COUKTOI
it. MKIWTATOI wwft surnr
12. ASM (CMOVAl STSHM
13. flfOnoSTAHC MK1P1TATOI
U. INOOCfO OlAfT ftM
15. STACK
14. KONOMIZtR
17. TOP Ol STtAM OIUM
II. SUPfl HfATfl
1*. LOWfl OIUM
20. raicio AII i NUT
                                         3-11

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disposed of in 10 foot layers and covered with soil.  A river is in
proximity to the landfill (i.e., approximately 100 yards).  There is no
leachate collection system, but there are four ground-water monitoring
wells.  Surface runoff is controlled with hay bales along the sides of
the landfill.  The two wells closest to the active area of the landfill
are often dry.  The two wells closest to the older portion of the
landfill contain water, but one well is at a very steep angle.
     3.2.3  Facility C
     The incinerator at Facility C includes two units, each consisting of
a reciprocating grate and a rotary kiln combustor.  The incinerator was
brought on line in January 1970, and currently a third unit is being added
to the facility.   The new unit will be equipped with a boiler and a
generator for energy recovery, and it should be operational by late 1986
or early 1987.  If the new unit is efficient and cost effective, then the
existing units will be retrofitted with energy recovery systems in the
future.  The two existing units are mass burn, volume reduction units
without resource recovery.  Figure 3.3 presents a diagram of the
incinerator.
     The existing units are identical, each having a rated capacity of
300 tons per day.   The actual operating capacity for each unit is
approximately 250 tons per day.  The units operate at approximately
1600°F to 1300°F,  and no additional fuel is used for burning the refuse.
The units have a residence time for combustion of 30 to 45 minutes.  Each
unit is equipped with a crude economizer to remove the coarse fly ash, a
cooling chamber to remove the medium fly ash, and an electrostatic
precipitator to remove the fine fly ash.
     The units are monitored in the control room to ensure that optimum
combustion efficiency is maintained.  The excess air, reciprocating grate
combustion chamber temperature, rotary kiln combustion temperature,
carbon monoxide,  feed rate, and residue generation are monitored.  The
feed rate and overfire air are continually adjusted to maintain efficient
operation.
                                   3-12

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                                                                                               Op (1C I
                                                                                               momt
lorccd   owtrhrc
droll  x-air
 ion      Ian
                                                                             rotary conveyers
                                                                               (lo  clurilier)
ESRcontrol
  room
                     Figure 3.3  Facility C Combustor

-------
     The feed to the units is approximately 50 percent residential and
50 percent industrial (i.e., paper,  wood,  plastics,  and metals).   The
facility does not process the waste  before combustion, however,  large
objects (e.g., tires, refrigerators, stoves, water heaters,  etc.)  are
removed by the feed crane operator,  if noticed.  The refuse  is gravity
fed into the incinerators; it has a  heating value of approximately 5000
BTU's per pound.  Each unit burns approximately 75,000 tons  of raw trasn .
per year.
     The residues from the combustors include bottom ash,  fly ash, and
quench water.  The units achieve a volume  reduction of 90  percent and a
weight reduction of 70 percent over  the raw refuse.   The bottom ash falls
into a quench water tank and is transported to a temporary storage bin by
a drag conveyor.  The fly ash is transported by a screw conveyor and a
trough to the quench water tank, where it  is removed with  the bottom
ash.  The displaced quench water overflows into a settling tank, where
the solids are removed.  The clarified quench water overflows a weir at
the end of the settling tank into a  wet well (i.e.,  sump),.and then
discharges to the local wastewater treatment plant.   "The bottom ash, fly
ash, and materials removed prior to  combustion are trucked to the on-site
landfill for disposal.
     The landfill is constructed as  a series of hills and valleys, where
the natural valleys are being filled with the combustion residues.  The
landfill has been used since 1970, and is  expected to be used until the
year 2050.  There is no leachate collection system, however, there is a
seep where field leachate may be collected.  The landfill is situated
very close to two streams.  The one stream  is fairly  small, and the
landfill actually extends over top of the stream with a culvert beneath
it.  The other stream is a major river approximately  300 yards away from
the landfill.  There are three monitoring wells and a production  well
located in between the landfill and river.  On a daily basis, waste  is
disposed by dumping the loads of residue on top, and  then pushing the
fresh loads down the sides with a bulldozer.
                                   3-14

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      3.2.4  Facility D
      The  Facility  0  incinerator  consists  of  two  identical water-wall
 traveling grate mass burn  combustors  similar to  the unit depicted in
 Figure  3.4.  The facility's  construction  began in December  1969,  and  the
 facility  began operating in  October 1972.  The units are rated  at 360 tons
 per day each, however,  the actual operating  capacity is approximately
 310 tons  per day for each  unit.  However,  if the refuse feed  is less  than
 5000 Btu's per pound,  the  feed rate is slowed to allow for  longer
 residence  times and  more complete combustion.  The units operate  24 hours
 per day,  7 days per  week,  50 weeks per year,  with approximately 2 weeks
 per year  for maintenance.  The units  typically operate at approximately
 1500 F, and no additional  fuel is used for the combustion.  The
 residence  times within  the units range from  4 to 5 hours with the longer
 residence  times necessary  for wet feed refuse.  The units are equipped
 with economizers and  electrostatic precipitators for removing fly ash.
 Steam is generated by the  progressive cooling of the furnace gases by the
 welded-membrane water-cooled walls of the combustion chamber, and by  the
 five  passes of the hot gases through  the convection and generating
 sections of the boiler.  Each boiler has a continuous steam generating
 capacity of 92,500 Ibs/hr.
     The units are monitored from a control  room using television
 monitors and operating variables.  The combustion temperature,  oxygen,
 feed  rate, and residue generation are all monitored.   Presently,  the
 combustion temperature is the major operational variable, however, the
 facility is switching to an oxygen monitoring system which was
 demonstrated to yield more  efficient operation.
     The feed to the units  is approximately 50 percent residential and
 50 percent industrial (e.g.,  wood,  paper, plastics, metals, etc.).
Additionally, in 1985 an automatad sludge disposal system was added to
permit the facility to incinerate sludge from the nearby wastewater
 treatment  plant.   The sludge  is mixed with the refuse, and the  feed rate
                                   3-15

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 is controlled  to maintain a combustion temperature of 1400°F to 1500*F.
 The facility does not process the waste prior to combustion, except that
 tires  are  removed and shredded before being burned.  However/ large
 noncombustible items (e.g./ refrigerators/ water heaters, etc.) are
 removed and sold for scrap metal.
     The residues from the facility include bottom ash, fly ash, and
 quench water.   The units achieve a volume reduction of 35 percent, not
 including  the  large materials removed before combustion.  Bottom ash
 falls  into a quench water tank and is transported by a conveyor belt to a
 temporary  storage bin.  Fly ash, which is removed by the economizer,
 drops  down a chute into the quench water tank.  The electrostatic
 precipitator ash is transported by a screw conveyor to the chute, where
 it  joins the economizer ash and is subsequently gravity fed to the quench
 water  tank.  The quench water is removed with the ash, and the overflow
 is  collected in a drain and routed to the wastewater treatment plant.
     Trucks transport the bottom ash, fly ash, and associated quench
 water  to the on-site landfill.  The landfill is a tall mound located on a
 square area (approximately 500'  x 500'}.  It has been in use for several
 years and  is now overflowing.   The landfill has a leachate collection
 system, however, the system is obstructed so leachate cannot be collected
 from this  system.   The facility does not have any ground water monitoring
 wells; it  is only approximately one mile east of a major river.
     3.2.5  Summary of Facility Design and Operating Characteristics
     Several differences and similarities, which may contribute to the
 residue characteristics, were  observed in the facility descriptions (see
 Sections 3.2.1. through 3.2.5) and are highlighted in this section.  All
 four incinerators  are less than 20 years old with capacities ranging from
 200 tons per day (tpd)  to 1120 tpd.   One of the incinerators is
 relatively small (Facility A-200 tpd), while the other three are of
medium size (600-1120 tpd).  Two of the incinerators are traveling or
 reciprocating grate  designs  (Facilities 3 and D); the third is a rotary
                                   3-17

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kiln design (Facility A); and the fourth is a combination of these two
designs (i.e., reciprocating grate and rotary kiln in series for
Facility C).  Large metal objects (e.g., water heaters,  refrigerators,
etc.) and tires are removed at each incinerator prior to combustion,
while only one incinerator (Facility A) processes its waste to remove
iron, aluminum, and .glass.  All four incinerators are equipped with
electrostatic precipitatocs to remove flue gas particulates, and two of
the incinerators (Facilities A and B) are also equipped with cyclones to
remove additional fly ash particles.  A summary of the design and
operating characteristics is presented in Taole 3.2
     The landfill for each facility is more than five years old and is a
monofill with only combustion residues and non-combustibles, including.
tires, disposed.  Three of the landfills (Facilities B,  C, and 0) are not
adequately lined or capped, and therefore, they would be expected to
produce and release leachates.  This is potentially a problem because the
landfills are generally close to the water table (<30 feet) and are in
proximity to surface water. .The fourth landfill (Facility A) is lined
and capped with clay, and therefore, does not pose a significant leachate
problem.  Three of the landfills are near capacity and are expected to
close by early 1987 (Facilities A, B, and D), while the fourth landfill
is expected to be used for at least 60 aore years.  Table 3.3 presents a
summary of the landfill characteristics.
     3.3  Samples and Sampling Procedures
     In order to meet the objectives of this study, Versar's personnel
collected MWC residue samples and field water samples from the four
facilities described in Section 3.2.  These samples were collected
between September 26 and October 22, 1936, and although the sampling
locations and techniques were facility specific, the samples from each
facility typically included:  bottom or combined ash, fly ash, quench
water, ground water, and field leachate.  Additionally, composite samples
of the fly and bottom ashes were collected for  laboratory extraction
                                   3-13

-------
                   TABLE 3.2  MUNICIPAL WASTE  COMBUSTOR DESIGN AND OPERATING CHARACTERISTICS
            Characteristic
      Facility A
   Facility B
    Facility C
Fac-ility 0
Hunter of Combustors
Designation of Each Combustor
Year of Construction
Energy Recovery System
Type of Combustor
Capacity (tons/day)
o Design
o Operating
Operating Schedule
Hours/day (days/week)
sign Combustion Temperature (F)
Residence Tim (hours)
Air Pollution Control System
2
n/tz
1981/1962
Yes
Continuous Feed
Water-wall
Rotary K1ln
100/100
75-90/75-90
24 (7)
1200
0.75
Cyclone, ESP
3
»2/f3/*4
1974/1974/1986
Yes
Continuous Feed
Water-wall
Traveling Grate
360/360/400
275/275/300
24 (7)
1300
0.75
Cyclone, ESP
2
»!/«
1970/1970
No
Continuous Feed
Reciprocating Grate
Rotary Kiln
300/300
250/250
24 (7)
1800
0.5 - 0.75
ESP
2
ll/»2
1972/1972
Yes
Continuous Feed
Water-wall
Reciprocating Grate
360/360
310/310
24 (7)
1400-1500
4 - 5
ESP
     Bottom Ash Handling System

      Fly Ash Handling System

    Quench Water Flow (gal/day)

       Quench Water Disposal

       Waste Composition (*)
          o Residential
          o Cornnerdal/Industrla!

  Waste Processing or Pre-handling
 Wet (Quench Tank)   Wet (Quench Tank)

 Wet (Quench Tank)          Dry

       17,000              35,000

        POTV                POTW
                  Wet (Quench Tank)   Wet (Quench Tank)

                  wet (Quench Tank)   Wet (Quench Tank)

                        23,000              23,000

                         POTW                POTW
         50
         50

   Remove large
 objects; separate
  glass, iron, and
aluminum for recyle
      80
      20

 Remove large
appliances and
    tires
       50
       50
    50
    50
Refuse Storage Location and Capacity     Piled in pit;       Piled in pit;
                                        two-day capacity    two-day capacity
  Large iten       Remove tires and
removed by crane  large noncombustible
    operator      materials: recycle
                   ferrous metals as
                  scrap; periodically
                  shred and burn tires

 Piled in pit;       Piled in pit;
two-day capacity    two-day capacity
                                                      3-19

-------
                                        TABLE 3.3  LANDFILL  CHARACTERISTICS
             Characteristic
 Amount of Combostor Residue Disposed
               (tons/day)

     Other Types of Waste Disposed
   Facility A
  Facility 8
    Facility C
  Facility 0
     Year Landfill  Began Operation

Projected Year Landfill  Reaches Capacity

                 Shape



       Lateral Dimensions (feet)

        Depth Below Grade (feet)

   Maximum Height Above  Grade (feet)

                 Slope



 Portion of Landfill  That is Capped (%)

       Cap Material and  Thickness


       Leachate Collection System


        Runoff Control Measures
60
Tires, large items.
construction
debris and.
noconbustibles
1982
1987
Rectangular


500 x 1. 000
<10
35 - 40
Relatively flat
with sloping
sides
90
Clay
3 feet
None

Impermeable cap;
graded contour;
diversion ditch
around landfill
perimeter
120
Large items and
construction debris


1981
1987
Rectangular


500 x I. 000
20
20
Relatively flat
with sloping
sides
90
Native soil
6-12 inches
None

Relatively thin
cap; hay bales
around one corner
of landfill to
inhibit runoff
155
Nonconbustlble
items


1970
2050
Rectangular
(multiple mounds
on hilly terrain)
300 x 1,500
0
60
Hilly terrain
with numerous
waste mounds
0
NA

None

Adjacent mounds
of waste tend
to trap surface
water; erosion of
slope evident
90
Tires and
noncombustibles


Post 1980
1987
Square


500 x 500
20
50
Single mound of
waste with steeply
sloped sides
0
NA

Gravel
(not functioning)
Flat area adjacent
to waste pi 1e
tended to collect
surface water

      Depth to Ground water (feet)

       Number of Monitoring Wells

   Distance to Nearest Domestic Well

   Distance to Nearest Surface water
       15
   10 - 15
2 (one useable)     4 (two useable)

   > 1/4 mile          < 500 feet
    200 fett
 (small stream)
   200 feet
(major river)
        30
1,000 - 1.500 feet

    1,000 fMt
  (major river)
     >100
  > 1/4 mile

    1 mile
(major river)
                                                        3-20

-------
 using three different leaching procedures (i.e./ Extraction Procedure,
 Toxicity Characteristic Leaching Procedure, and Mono-filled Waste
 Extraction Procedure).  Where available, samples of disposed ash and
 discrete fly ash fractions were also collected to more adequately
 characterize the MWC residues and the environmental effects of their
 disposal.  The following sections (See Sections 3.3.1 through 3.3.4) will
 describe, in detail, the samples, sampling locations, and sampling
 procedures for each of the four facilities.
     3.3.1  Facility A
      Versar personnel collected groundwater samples at Facility A's
 landfill on September 25, 1986 and MWC residue samples at Facility A on
 September 26, 1986.  The MWC residue samples included:  bottom/fly ash
 (i.e., a mixture of bottom ash and fly ash), fly ash, and quench water.
 As per sampling plan specifications, 25 percent of the samples were
 collected in duplicate for quality control (QC).
     The MWC residue sampling at Facility A commenced at the beginning of
 the second shift (i.e.,  7:00 a.m. to 3:00 p.m.) on Friday, September 26,
 1986, and was completed at the end of the third shift (i.e., 3:00 p.m. to
 11:00 p.m.)  on Friday, September 26, 1986.
     Units 1 and 2 were  sampled separately to determine if any
 differences  exist in the characteristics of the residues due to the
 independent  operating parameters for each system.
     Although the landfill at Facility A did not have a leachate
 collection system, the Versar monitoring team explored the perimeter of
 the landfill to find a natural seep for leachate collection.  Such a
 location did not exist,  so no field leachate samples were collected.
 However, at  the request  of EPA/HWERL, a follow-up visit was scheduled for
 October 22,  1986, to again attempt to collect a field leachate sample.
Although the follow-up visit was scheduled after a period of heavy rain,
 the landfill perimeter was still dry with no natural seeps.  Therefore,
no field leachate samples could be obtained at Facility A.
                                   3-21

-------
     While  the  samples were being collected, the combustor operator
 recorded pertinent operating data to be used for evaluating contaminant
 concentration differences between units, shifts, and facilities  (See
 Section 5.0).   This operating data is shown in Section 4.1, Table 4.1.
 Table  3.4 presents a summary, including field sample numbers, of the
 samples collected at this facility.  Detailed descriptions of the
 sampling locations and procedures for each of the sample matricies are
 presented below.
     Groundwater - The groundwater samples were grab samples collected
 the afternoon of September 25, 1986.  There are two groundwater
 monitoring wells in the section of the landfill near where the ash is
 placed.  One monitoring well that is closer to the older ash was dry.
 The second monitoring well which is closer to the freshly placed ash, is
 on a hillside approximately 400 to 500 feet from the active part of the
 landfill and contained water.
     Prior to sampling the groundwater in the second monitoring well, the
 volume of standing water in the well casing and saturated annulus was
 determined by measuring and recording the well casing diameter, the depth
 from the top of the well casing to the water surface, and the depth from
 the top of the well casing to the sediment/water interface.  The volume
of standing water was approximately 0.3 gallons.
     Because of the small volume of water and the reported slow
 recharging rate, the monitoring well was not evacuated.   Instead, grab
samples were collected from the standing water using a Teflon bailer.
The water was clear with no visible particulate matter;  therefore, the
samples were not filtered.  The clean, labeled sample containers (i.e.,
4-oz.  glass for TOG,  1-L glass for organic scan,  1-L plastic for metals,
and one and a half 1-L glass for PCDO/PCDF) were filled directly from the
Teflon bailer,  documented on chain-of-custody forms, packed on ice in an
Igloo-type cooler,  and shipped to the laboratory by priority air express.
The coolers were secured with EPA custody seals.
                                   3-22

-------
                                  TABLE 3.4  SAMPLE IDENTIFICATION COOES FOR  FACILITY A
  Sample
  Matrix

  Blank
  Sample
Description

Trip Blank
Bottom/Fly        Composite
Bottom/Fly    Unit 1, 9/26, AN
Bottom/Fly    Unit 1. 9/26, PN
Bottom/Fly    Unit 2. 9/26, AN
Bottom/Fly  Unit 2. 9/26. AM, Oup
Bottom/Fly    Unit 2, 9/26. PN

   Fly            Composite
   Fly         Composite, Oup
   Fly        Unit 1, 9/26, AN
   Fly      Unit 1. 9/26, AN, Oup
   Fly        Unit I. 9/26, PN
   Fly        Unit 2. 9/26, AN
   Fly        Unit 2. 9/26, PN

  MHell               II

  Quench        Unit 1,  9/26
  Quench        Unit 2,  9/26
       Organic
TOC     Scan    Metals      SNA         PCS
No.      No.      No.        No.          No.

17652    17653    17650   17654-57    17662-63
                                      17626                   17625
                                      17639                   17640
                                      17618                   17619
                                      17621                   17622
                                      17633                   17634
                                      17627                   17628
                                      17630                   17631
                                      17636    .               17637
                                      17642                   17643
                                      17645                   17646

                    18363    17506    18370

                    18362    17504    17501    17538-41    17546-47
                    18375    17505    18369    17548-51    17556-57
PCOO/
 PCOF
 No.
   Lab
Leachate
   No.
   17658
                                                      17624
                                                      17641
                                                      17620
                                                     17623"
                                                      17635
                                                      17629
                                                      17632
                                                      17638
                                                      17644
                                                      17647

                                                17523-24-

                                                 17542-45
                                                 17552-55
                                                                                   17651
                                                                                   17648
                                                                                   17649
                   LEGEND:
                                  Bottom/Fly -  Combined bottom ash and fly ash samples
                                  Fly • Fly ash
                                  MHell • Groundmter  from monitoring well
                                  Quench • Incinerator quench water
                                  TOC - Total organic  carton
                                  SNA • Base/neutral acid extractable organic*
                                  * • Sample collected but not analyzed
                                                 3-23

-------
     Bottom/fly ash - The Versar monitoring team collected a combined ash
 (i.e., a mixture of-bottom ash and fly ash) sample rather than a bottom
 ash sample because a location where a discrete bottom ash sample could be
 collected was not available.  Each bottom/fly ash sample was a
 time-composite composed of eight grab samples representing each
 combustor/shift combination (i.e.. Unit 1 or Unit 2, 2nd shift or 3rd
 shift).
     During the 2nd shift, the grab sample portion of the time-composite
 sample was collected every hour over an eight-hour period.  Unit 1 was
 having a clinker problem and Unit 2 was naming raw refuse.  The fourth
 grab sample from Unit 2 was collected after a 1-1/2 hour interval rather
 than a 1-hour interval because the drag conveyor had been shut off.  The
 seventh grab sample from both units was collected after a 2-hour interval
 during which the Unit 2 conveyor had been shut off for about an hour.
 During the 3rd shift, sample increments were collected every 45 minutes
over a five and one half-hour period.   At the beginning of shift 3,
Unit 1 was burning hot and the bottom ash on the conveyor was on fire/-
therefore. Unit 1 was not sampled for the first three grabs and the
volume of the last five grabs was doubled.  Unit 2 was still running
cold.   Per sampling plan requirements, the time-composite collected from
Unit 2 during the second shift was split for field and laboratory control.
     Each bottom/fly ash grab sample was collected from the quench tank
drag conveyor of each unit.   The drag conveyor transports the ash from
the quench tank up an incline to a storage bin.   As the ash is conveyer
up the incline, the quench water returns down the slope to the quench
tank.   The bottom/fly ash is wet and contains uncombusted material (e.g.,
glass, cans,  and metal scraps).
     Each sample increment of the time-composite sample was collected by
stopping the  drag conveyor and by taking a stopped-belt cut (ASTM
Method D2234-76) across the conveyor using a steel shovel.  The cut was
perpendicular to the conveyor direction and was the width of the shovel.
The sides of  the cut were as nearly parallel as possible to prevent
                                   3-24

-------
 particle-size bias.  The incremental sample was placed in a polyethylene
 lined three-gallon collection bucket and was thoroughly mixed with a
 steel hand  trowel.  A 550-milliliter subsarcple (1,100 milliliters for the
 sample to be split) was transferred to a lined compositing bucket.  Large
 pieces of uncombusted material were not included in the samples to
 prevent sample bias.
      At the end of the sampling period, the material in the compositing
 bucket was thoroughly mixed with a hand trowel.  The time-composite
 sample was placed into clean, labeled sample containers (i.e., one
 1-quart glass wide-mouth jar each for PCDD/PCDF, PCS, and metals) using a
 steel  hand trowel.  In addition, the polyethylene bottle used to measure
 the 550-milliliter aliquots was filled to obtain the bottom/fly ash
 composite sample for laboratory leachate testing.  The laboratory
 leachate composite was prepared such that it is representative of both
 combustors and both shifts of operation during which sampling was
 performed.  The samples were documented on chain-of-custody forms, packed
 in Igloo-type coolers without ice, and shipped to the laboratory by
 priority air express.  The coolers were sealed with EPA custody seals.
     Fly ash - Similar to the bottom/fly ash samples, four time composite
 fly ash samples were collected composed of eight grab samples each
 representing each combustor/shift combination (i.e.. Unit 1 or Unit 2,
 2nd shift or 3rd shift).   The fly ash samples were taken at the same
 frequencies as the bottom/fly ash samples during the 2nd and 3rd shifts.
The volume of the fourth grab sample from Unit 2 was half the usual
amount, because Unit 2 was running cold.   Per sampling plan requirements,
the fly ash time-composite collected from Unit 1 during the 2nd shift was
 split for field and laboratory quality control.
     Each fly ash grab sample from Unit 1 was collected from a screw
conveyor and each fly ash grab sample from Unit 2 was collected at the
 inlet to a turbulator.   For each unit,  screw conveyors transport the fly
ash from separate cyclone separators and electrostatic precipitators to
                                   3-25

-------
turbulators where water is added.  The fly ash slurry feeds to the quench
tank displacing some quench water.
     The grab samples from Unit 1 were collected by placing a steel hand
trowel under the discharge of the screw conveyor and collecting a full-
stream cut (ASTM Method D2234-76).  The full-stream cut was collected by
placing the steel hand trowel under tr.e screw conveyor discharge, allowing
it to fill up, transferring the material to a polyethylene lined three-
gallon bucket and repeating several times until sufficient material was
collected.
     The grab samples from Unit 2 were collected by placing a steel hand
trowel under the inlet of the turbulator.  The part-stream cut (ASTM
Method 02234-76) was collected by placing the steel hand trowel under the
turbulator inlet, allowing it to fill up, transferring the material to a
polyethylene lined three-gallon bucket, and repeating several times until
sufficient material was collected.
     After each grab sample was collected, the sample was thoroughly
mixed with the steel hand trowel, and a 550-milllliter aliquot
(1100-milliliters for samples to be split) measured into a polyethylene
bottle and poured into a covered and lined 3-galIon compositing bucket
until the end of the shift.
     At the end of the compositing period, the material in the
compositing bucket was homogenized identically to the bottom/fly ash and
placed into clean, labeled sample containers (i.e., one 1-quart glass
wide-mouth jar each for PCDD/PCDF, PCB, and metals).  In addition, the
polyethylene bottle used to measure the 550 milliliter aliquots was
filled to obtain the fly ash composite sample for laboratory leachate
testing.  The laboratory leachate composite was prepared such that it is
representative of both combustors and both shifts of operation during
which sampling was performed.  Per sampling plan requirements, the
laboratory leachate was split for field and laboratory control.  The
samples were documented on chain-of-custody forms, packed in Igloo-type
                                   3-26

-------
 coolers without ice,  and shipped to the  laboratory by priority  air
 express.  The coolers were secured with  EPA  custody seals.
      Quench water - The quench water samples were  grab samples
 representing one combustor (i.e..  Unit 1 or  Unit 2).  The samples were
 collected during the  second shift  (i.e.. Unit  1 quench water collected
 about half way through the shift and Unit  2  quench water collected
 towards the end of the shift).   This being the case, these  samples were
 not  representative of the entire shift,  but  only the instant in time at
 which they were collected.   Therefore, any time dependent variability of
 the  quench water contaminant concentrations  was not accounted for in
 these samples.
      The quench water samples were  collected in the tank.  The  fly ash
 slurry from the turbulator feeds to the  quench tank displacing  some
 quench water.   The displaced quench water  overflows to a sump where
 solids are removed.   The  effluent from the sump is  discharged to the
 sanitary sewer.   The  quench water samples  were collected in the tank
 rather than at  the sump overflow because the sump overflow was  not
 accessible.
      The  quench water grab  samples  were  collected using a clean sample
 container (i.e.,  4-oz. glass for TOG, 1-L  polyethylene for metals,
 1-L glass  for organic scan,  four 1-L glass for base/neutral/acid, two
 1-L glass  for PCB,  and four  1-L glass for  PCDD/PCDF).  The samples were
 treated with the  appropriate preservative  (i.e., sulfuric acid  for TOC
 and organic scan,  and nitric acid for metals), documented on chain-of-
 custody forms, packed on  ice in Igloo-type coolers, and shipped to the
 laboratory by priority air express.  The coolers were secured with EPA
 custody seals.
      3.3.2  Facility B
     Versar personnel collected groundwater samples at Facility B's
 landfill on September 27, 1986, and MWC residue samples at Facility B on
September 28 and 29, 1986.  The MWC residue samples included:  bottom
                                   3-27

-------
ash, fly ash, and quench water.   Per sampling plan,  25 percent of the
samples were collected in duplicate for quality control (QC).
     The MWC residue sampling at Facility B was performed during the
second shift (i.e., 7:00 a.m. to 3:00 p.m.) on Sunday, September 23, 1986
and the third shift (i.e., 3:00  p.m. to 11:00 p.m.)  on Monday,
September 29, 1986.  The reason  for the length of time between each
sampling shift was to determine  if any differences exist in the
characteristics of the residues  due to the length of time the  refuse has
been in the incoming refuse collection pit.  During sampling,  Unit 2 was
down for maintenance; therefore, all MWC residue samples were  collected
from combustion Units 3 and 4.  Units 3 and 4 were sampled separately to
determine if any differences exist in the characteristics of the residues
due to different operating parameters and incinerator design features.
     Although the Versar monitoring team also attempted to collect a
field leachate sample, no natural leachate seeps were available for
collection.  However, at the request of EPA/HWESL, a follow-up visit was
scheduled for October 22, 1986,  to attempt collection of a field leachate
sample.  The follow-up visit was scheduled after periods of heavy rain;
therefore, Versar personnel were able to collect three field leachate
samples during this visit.
     While the samples were being collected, the combustor operator
recorded pertinent operating data to be used for evaluating contaminant
concentration differences between units, shifts, and facilities (See
Section 5.0).  This operating data is shown in Second 4.1, Table 4.2.
Table 3.5 presents a summary, including field sample numbers,  of the
samples collected at this facility.  Detailed descriptions of the
sampling locations and procedures for each of the sample matricies  are
presented below.
     Groundwater - The groundwater samples were grab samples collected
the afternoon of September 27, 1986.  There are four groundwatar
monitoring walls at the landfill.  The two wells closest to the active
                                   3-28

-------
               TABLE 3.5  SAMPLE IDENTIFICATION  COOES  FOR FACILITY B
Sample
Matrix
Blank
Bottom
Bottom
Bottom
Bottom
Bottom
Bottom
Fly .
Fly
Fly
Fly
Fly
Fly
Leachate
leactiate
Leachate
MWell
Quench
Quench
Quench
Sample
Description
Trip Blank
Composite
Unit 3. 9/28. AH
Unit 3, 9/29, PM
Unit 4. 9/28, AM
Unit 4, 9/28, AM, Oup
Unit 4. 9/29. PM
Composite
Unit 3, 9/28, AM
Unit 3, 9/28, AM, Oup
Unit 3, 9/29, PM
Unit 4, 9/28, AM
Unit 4, 9/29, PM
East Side
North Side
Northeast Corner
12
Unit 3. 9/28
Unit 4, 9/28
Unit 4, 9/28, Oup
                         Organic
                  TOC     Scan    Metals      SNA          PCS
                  No.      NO.      NO.        No.          Ho.
PCOO/       Lab
 PCOF    Leachate
 No.        No.
                  17696    17698    17697   17699-02    11703-04     17705-08
                                                                                 17694










19830
19856
19843
18367
18376
18377
18364










19832
19858
19845
17512
17S09
17510
17508
17664
17688
17673
17676
17682
17667
17670
17691
17679
17685
19831
19857
19844
18373
17502
17503
18371










19833-36
19861-64
19848-51
17579-80-
17588-91
17598-01
17528-31
17666
17690
17674
17677
17683
17669
17672
17693
17680
17686
19837-38
19859-60
19846-47

17596-97
17606-07
17536-37
17665
17689
17675
17678
17684
17668
17671
17692
17681
17687
19839-42
19865-68
19852-55
17582-85*
17592-95*
17602-05
17532-35
                                                                                17695
LEGEND:
               8otto» • Bottom ash
               Fly - Fly ash
               MMtll • Groundwater from monitoring well
               Quench • Incinerator quench  water
               TOC • Total  organic carbon
               SNA « Base/neutral  add ax tractable organlcs
               * • Samples  collected but not  analyzed
                                3-29

-------
area of the landfill were in poor condition (one had been damaged by a
vehicle) and were dry.  The two wells closest to the older portion of the
landfill contained water, but one well casing was at a very steep angle
and an accurate reading could not be obtained for the depth of the water
surface.
     Prior to sampling the groundwater in the one remaining well, the
volume of standing water in the well casing and saturated annulus was
determined by measuring and recording the well casing diameter, the depth
from the top of the well casing to the water surface, and the depth from
the top of the well casing to the sediment/water interface.  The volume
of standing water was approximately 2.6 gallons.
     Because of the small volume of water and uncertainty on the
recharging rate, the monitoring well was not evacuated.   Instead, grab
samples were collected from the standing water using Teflon bailers.  The
water was clear with no visible particulate matter;  therefore, the
samples were not filtered.   The clean labeled sample containers (i.e.,
4-oz.  glass for TOC, 1-L polyethylene for metals, 1-L glass for organic
scan,  one and three quarter 1-L glass for base/neutral/acid, a-nd four
1-L glass for PCDO/PCDF) were filled directly from the Teflon bailer,
documented on chain-of-custody forms, packed on ice  in an Igloo-type
cooler, and shipped to the laboratory by priority air express.  The
coolers were sealed with EPA custody seals.
     The Versar monitoring team returned to the Facility B landfill on
September 28,  1986, to determine how well the monitoring well recharged.
Unfortunately,  the volume of standing water had not  increased
significantly,  so no more samples were taken.
     Bottom ash - The bottom ash samples were composite samples composed
of four grab samples representing each combustor/shift combination  (i.e..
Unit 3 or Unit  4,  2nd shift on September 28, 1986 or 3rd shift on
September 29,  1986).  Unit 4 was running below optimum temperature  during
the beginning of the third shift on September 29, 1986.  A grab sample
                                   3-30

-------
 portion of the  composite  was  collected  each  time  bottom ash was
 transferred to  a  dump truck during  the  shift.  Per  sampling plan
 requirements, the composite collected from Unit 4 during  the second shift
 on September 29,  1986 was split  for field and  laboratory  quality  control.
      Each bottom  ash  grab sample was collected from a disposal trailer.
 The bottom ash  is spray quenched, stored in  an enclosed hopper, and
 discharged into a disposal trailer  about every two  hours.  Each trailer
 has sufficient  capacity to hold  two bottom ash dumps.  During the
 sampling visit. Unit  3  was dumped in the back  half  of the trailer and
 Unit 4  was dumped in  the  front half.
      The grab sample  portion  of  the composite  sample was  collected  by
 climbing up on  the trailer and scooping with a steel hand trowel several
 aliquots of ash from  the  freshly dumped mound and placing the material in
 a  polyethylene  lined  three-gallon collection bucket.  The sample was
 thoroughly mixed  with the  steel  hand trowel, and  a  1-quart aliquot
 (2-quart for the  sample to be split) was transferred into a polyethylene
 covered and lined 3-gallon compositing bucket until the end of the
 shift.   Large pieces  of uncombusted material were not included in the
 samples  to prevent sample  bias.
     At  the end of the sampling  period, the material in the compositing
 bucket was  thoroughly mixed with a hand trowel.  The composite sample was
 placed  into clean, labeled sample containers (i.e., one 1-quart glass
 wide-mouth jar each for PCDD/PCDF, PCB, and metals  (using a steel hand
 trowel.  The polyethylene  bottle used to measure the 1-quart aliquots was
 filled to  obtain the  bottom ash  composite sample for laboratory leachate
 testing.  The laboratory leachate composite was prepared such that  it is
 representative of both combustors and both shifts of operation during
which sampling was performed.   The samples were documented on chain-of-
custody  forms,  packed in Igloo-type coolers without ice, and shipped to
the laboratory by priority air express.   The coolers were sealed with EPA
custody  seals.
                                   3-31

-------
     Fly ash - Similar to the bottom ash samples, the fly ash samples
were composites composed of four grab samples representing each combustor/
shift combination (i.e.. Unit 3 or Unit 4, 2nd shift on September 28,
1986, or 3rd shift on September 29, 1986).  An incremental sample portion
of the composite was collected at times corresponding to periods when
bottom ash was dumped during the shift.  Per sampling plan requirements,
the composite collected from Unit 3 during the second shift on September
29, 1986, was split for field and laboratory quality control.
     Each fly ash grab sample was collected from a screw conveyor.  The
fly ash from each unit is removed from the flue gas stream in separate
cyclones and electrostatic precipitators, mechanically conveyed (i.e.,
screw conveyors) to a combined duct, and discharged to an enclosed
storage bin through a large hose.
     The grab samples were collected by turning the screw conveyor off,
removing the screw conveyor cover, and collecting the exposed material
with a gloved hand.   The collected material was placed in a polyethylene
lined three-gallon bucket.
     After each grab sample was collected, the sample was thoroughly mixed
with the steel hand trowel, and a 1-quart aliquot (2-quart for a sample
to be split) transferred to a polyethylene bottle and poured into a
polyethylene covered and lined 3-gallon compositing bucket until the end
of the shift.
     At the end of the compositing period, the material in the compositing
bucket was homogenized and placed into clean, labeled sample containers
(i.e.,  one 1-quart glass wide-mouth jar each for PCDD/PCDF, PCS, and
metals).   In addition, the polyethylene bottle used to measure the
1-quart aliquots was filled to obtain the fly ash composite sample for
laboratory leachate  testing.   The laboratory leachate composite was
prepared such that it is representative of both combustors and both
shifts of operation during which sampling was performed.  The samples
were documented on chain-of-custody forms, packed in Igloo-type coolers
                                   3-32

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 without ice, and shipped to the laboratory by priority air express.   The
 coolers were sealed with EPA custody seals. •
      Quench water - The  quench water samples  were  grab samples
 representing one combustor (i.e..  Unit  3  or Unit 4).   The  samples  were
 collected during the second shift  on September 23,  1986 (i.e..  Unit  4
 quench water collected at the beginning of the shift  and Unit 3 quench
 water collected  about half way through  the shift).  This being  the case,
 these samples were  not representative of  the  entire shift,  but  only  the
 instant in time  at  which they were collected.   Therefore,  any time
 dependent variability of the  quench  water contaminant  concentrations  was
 not  accounted for in these samples.   Per  sampling  plan requirements,  the
 grab samples  for Unit 4  were  split for  field  and laboratory quality
 control.
      The  quench  water grab samples were collected  below the bottom ash
 clamshell  load-out  hoppers.   The bottom ash is  spray quenched and  stored
 in an enclosed hopper.   Quench water  drains from the bottom ash hoppers,
 spills  to  the pavement below,  and  is  collected  in  a surface drain.  The
 quench  water  is  discharged to  the  sanitary sewer after  solids are  removed
 in a  sump.  The  quench water  samples  were collected below the bottom  ash
 hopper  because the  sump  overflow was  not accessible.
     The quench  water grab  samples were collected using  a 2-1/2  gallon
 wide-mouth glass jar.  The  2-1/2 gallon jar was filled  several  times  to
 obtain  sufficient volume for analysis (i.e., 3 times for Unit 4  and 2
 times for Unit 3).  The contents of the 2-1/2 gallon jar was poured into
 clean labeled sample containers (i.e., 4-oz. glass for TOO, 1-L
 polyethylene for metals,  1-L glass for organic scan, four 1-L glass for
 base/neutral/acid, two 1-L glass for  PCS and four 1-L glass for
 PCDD/PCDP).  The samples  were treated with the appropriate  preservative
 (i.e., sulfuric acid for TOG and organic scan, and nitric acid  for
metals), documented on chain-of-custody forms, packed on ice in
 Igloo-type coolers,  and shipped to the laboratory by priority air
express.  The coolers were secured with EPA custody seals.
                                   3-33

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     Field  leachate - Three field leachate samples were collected during
 the follow-up visit to Facility B on October 22, 1986.  These field
 leachates were grab samples collected from tne northeast corner and the
 north and east sides of the landfill.  All three of these samples were
 collected along the bottom edge of the landfill, where natural leachate
 seeps flowed out from underneath the landfill.  The seeps then flowed
 through a culvert, underneath the road, into a nearby river.  The
 discharge point of the leachate seeps into the river was observed without
 noting any deleterious effects.
     The natural seep streams at all three sampling locations were too
 shallow to collect a representative sample without disturbing the
 sediment.  Therefore, the Versar monitoring team used a shovel to dig a
 sample collection basin in the leachata scream flow channel.  Before the
 samples were collected, the leachate stream was allowed to fill the
 basin,  and the sediment was allowed to settle.  After the leachate filled
 the basin and was clarified,  the samples were collected using a
 borosilicate glass beaker and transferred to the appropriate, precleaned
 sample containers. -Then, the samples were labeled, documented on
 chain-of-custody forms, packed in coolers, iced, and shipped to the
 laboratory by priority air express.
     3.3.3  Facility C
     Versar personnel collected MWC residue samples at Facility C between
September 23, 1986, and September 30, 1986.  These samples included:
bottom/fly ash (i.e., a mixture of bottom ash and three discrete fly ash
fractions),  fly ash (i.e., a  mixture of the three discrete fly ash
fractions),  quench water, coarse fly ash (i.e., economizer ash), medium
fly ash (i.e.,  cooling chamber ash), fine fly ash (i.e., electrostatic
precipitator dust), disposed  ash, and ground water (i.e., water from the
facility's production well).   Per sampling plan requirements, 25 percent
of these samples were collected in duplicate for quality control (QC)
purposes.
                                   3-34

-------
     The sampling plan for this facility stipulated that Versar personnel
would also collect field leachate and additional ground water samples.
However, the Versar monitoring team was unable to obtain these samples
during this visit.  Although evidence of a natural leachate seep was
observed below the landfill, it was dry.  Nevertheless, the Versar
monitoring team did observe some surface water runoff (i.e., possibly
field leachate) from the landfill, but the runoff stream was extremely
shallow with a minimal flow volume.  Therefore, adequate sample volumes
(approximately three gallons would be required) could not be collected.
Furthermore, because of the extremely shallow depth of the runoff stream,
a representative sample could not be collected without disturbing the
sediment (i.e., disposed ash) over which the runoff was flowing.
     The additional groundwater samples were to be collected from three
on-site monitoring wells.  However, two of these wells were locked, and
all three wells were equipped with dedicated compressed air pumps (i.e.,
Well Wizards).   The Versar monitoring team was unable to gain access to
the keys or the pump operating equipment, and as a result, the wells were
not sampled.
     However,  at the request of EPA/HWERL, a follow-up visit was scheduled
for October 21, 1986, to obtain the field leachate and monitoring well
samples.   Prior to the follow-up visit, Versar contacted the facility's
monitoring well installation and sampling contractor to ensure that the
keys and pumping equipment would be available for sampling.  Therefore,
the three ground water samples were collected during this follow-up
visit.   Furthermore,  because the follow-up visit was scheduled after a
period of heavy rain, Versar was also able to collected three field
leachate  samples.
     The  MWC residue  sampling at Facility C commenced during the second
shift (i.e., 3:00  p.m.  to 11:00 p.m.) on September 28, 1986, and was
completed at the end  of the second shift on September 30, 1986.  During
these sampling  activities.  Unit 1 was down for maintenance; therefore.
                                   3-35

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all MWC residue samples were collected from combustion Unit 2.  While the
samples were being collected, the incinerator operator recorded pertinent
operating data to be used for evaluating contaminant concentration
differences between shifts and facilities (see Section 5.0).
This operating data is shown in Section 4.1, Table 4.3. Table 3.6 presents
a summary, including field sample numbers, of the samples collected at
this facility.  Detailed descriptions of the sampling locations and
procedures for each of the sample matricies are presented below.
      Bottom/fly ash - The Versar monitoring team had to collect a
combined ash (i.e., bottom and fly ash mixture) rather than a bottom ash
sample because a discrete bottom ash sampling location was not
available.  The bottom/fly ash sample included all the ash types
generated by the facility (i.e., bottom ash, coarse fly ash, medium fly
ash, and fine fly ash).   These bottom/fly ash samples were
time-composited samples representing one shift of operation and one
combustion unit (i.e.. Unit 2).   Initially, the discrete grab sample
portions of the composite were cpllected each hour over an eight-hour
period, and then manually composited at the end of this period.  However,
because of the time required to composite and containerize (including
chain-of-custody documentation,  labeling, and preservation) the samples,
the sampling increment was changed to every 40 minutes over a six-hour
period.
     Each discrete bottom/fly ash grab sample was collected from the
quench water tank drag conveyor.  The drag conveyor exited the quench
water tank and transported the ash up an inclined surface to a load-out
bin, where the ash was discharged into a truck for subsequent disposal.
As the ash was conveyed up the slope, the water returned down the slope
to the quench water tank.  However,  the ash was still very wet and
contained a large amount of uncombusted material (e.g., glass, cans,
metal scraps, etc.).
     The sample increments were collected by stopping the drag conveyor
and taking a stopped-belt cut (ASTM Method D2234-76) across the conveyor
                                   3-36

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                                  TABLE 3.6  SAMPLE IDENTIFICATION CODES FOR FACILITY C
  Sample
  Matrix

  Blank
  3 lank-
   Description

   Field Blank
   Trip Blank
Bottom/Fly        Composite
Bottom/Fly     Composite. Oup
Bottom/Fly    Unit 2. 9/28. PM
Bottom/Fly    Unit 2. 9/29. PM
Bottom/Fly    Unit 2. 9/30. AM
Bottom/Fly  Unit 2. 9/30. AM. Oup
Bottom/Fly    Unit 2, 9/30. PM

   Fly            Composite
   Fly        Unit 2, 9/28, PM
   Fly        Unit 2. 9/29. PM
   Fly      Unit 2. 9/29. PM. Oup
   Fly        Unit 2, 9/30, AM
   Fly        Unit 2, 9/30, PM
   Fly         Unit 2. Coarse
   Fly       Unit 2. Fine (ESP)
   Fly         Unit 2, Medium

 Landfill    Perimeter Composite
 leachate
 Leachate
 Leachate

  HWell
  MWell
  MWell
  PWell

  Quench
  Quench
   North Side
Northeast Corner
Northwest Corner
       #3
       M
 Production Hell

  Unit 2. 9/28
  Unit 2. 9/30

TOC
No.
19592
19537

















19803
19791
19815
19778
19753
19766
19581
19512
19568
Organic
Scan
No.

19535

















19829
19828
19827
19780
19754
19767
19578
19511
19569

Metal j SNA
NO. No.

19536 19525-28


19514
19539
19586
19589
19593

19518
19542
19545
19583
19596
19548
19554
19551
19522
19804 19811-14
19792 19795-98
19816 19823-26
19779 19781-84
197S2 19755-58
19765 19768-71
19582 19570-73*
19513 19501-04*
19557 19558-61

PC8
No.

19533-34


19515
19540
19588
19591
19595

19519
19543
19546
19585
19598
19549
19555
19552
19523
19805-06
19793-94
19817-18
19785-66
19759-60
19772-73
19579-30
19509-10
19566-67
PCDO/
PCDF
No.

19529-32


19516
19541
19587
19590
19594

19520
19544
19547
19584
19597
19550
19556
19553
19524
19807-10
19799-02
19819-22
19787-90*
19761-64*
19774-77*
19574-77*
19505-08
19562-65
Lab
Leachate
No.


19517
19517D





19521


















                   LEGEND:
                                  Bottom/Fly • Combined bottom ash and  fly ash samples
                                  Fly - Fly ash
                                  MWell • Groundwater from monitoring well
                                  PWell - Groundwater from production well
                                  Quench - Incinerator quench  water
                                  TOC • Total organic carbon
                                  SNA • Base/neutral  add ex tractable organ 1cs
                                  • • Samples collected but not analyzed
                                                  3-37

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bar using a shovel.   The cut was perpendicular to the conveyor direction
and was the width of the shovel.  The sides of the cut were as nearly
parallel as possible to prevent particle-size bias.   The sample was
placed in a three-gallon container and covered with polyethylene sheeting
to prevent contamination during compositing.
     At the end of the compositing period,  the material in the bucket was
poured into a polyethylene bag and thoroughly mixed by inverting the bag
several times.   Before the sample was containerized, large pieces of
uncombusted material were removed to prevent sample bias.   Then, the
homogeneous material was placed into clean sample containers (i.e., one
glass wide-mouth quart jar for each PCDD/PCDP, PCS,  and metals sample)
using a small steel  garden trowel, and the samples were labeled  and
documented on chain-of-custody forms.  An additional wide-mouth jar was
filled 1/4 of the way to obtain the bottom/fly ash composite sample for
laboratory leachate  testing.  This laboratory leachate composite sample
was prepared such that it is representative of the four shifts of
operation during which sampling was performed.
     The four bottom/fly ash composite samples and the one bottom/fly ash
laboratory leachate  composite were collected during the second shifts on
September 23 and 29, 1986, and the first and second shifts on
September 30, 1986.   Additionally, per sampling plan requirements, one of
these samples (i.e., first shift on September 30, 1986) was collected in
duplicate for field  and laboratory quality control.   The containerized
samples were packed  on ice in Igloo-type coolers and shipped to the
laboratory by priority air express.
     Fly ash - Similar to the bottom/fly ash samples, the fly ash samples
were time composites representing one shift of operation and one
combustion unit.  Also like the bottom/fly ash samples, the fly ash
sampling frequency was changed from every hour for an eight-hour period
to every 40 minutes  for a six-hour period.  At Facility C, there were
three discrete fly ash fractions that had to be collected individually
                                   3-38

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 and than manually composited.  These three fractions were the coarse fly
 ash, medium fly ash, and fine fly ash.
     The coarse fly ash particles settle out of the flue gas stream in
 the economizer.  The economizer functions by forcing the flue gas through
 a series of bends which decrease the stream's velocity.  This causes the
 larger particles to settle out of the stream because they become too
 heavy for the decreased velocity.  These settled particles fall down a
 chute into a sloped quench water trough, where they are carried to the
 quench water tank.
     This coarse fly ash fraction was collected at the discharge of the
 chute.  The sample increments were collected by using a one pint
 container to collect a full-stream cut.  The full-stream cut was
 collected by placing the container underneath the discharge of the chute
 and allowing it to fill.  The sample was placed in a three-gallon bucket
 and covered with polyethylene sheeting to prevent contamination while the
 medium fly ash was being collected.
     The medium fly ash particles were removed from the flue gas stream
 in a cooling chamber.   As -the flue gas enters the chamber, cooling water
 is sprayed on the gas  stream to reduce the temperature and to remove
additional fly ash particles.  Then, the cooling water and ash particles
descend through the cooling chamber to a small holding tank at the head
of the quench water trough.  Finally, the water and ash particles overflow
 the tank and flow down the quench water trough to the quench water tank.
     This medium fly ash fraction was collected from the holding tank
before it overflowed into the trough.  The sample increments were
collected by thoroughly mixing the contents of the holding tank with a
shovel,  and then removing approximately one pint of sample, using the
shovel,  and placing the sample in the three-gallon bucket with the coarse
fly ash fraction.   Again,  the bucket was covered with polyethylene
sheeting while the fine fly ash fraction was being collected.
                                   3-39

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      The fine  fly ash particles were  removed from the flue gas stream  in
 the final pollution control device, an electrostatic precipitator  (ESP).
 The ESP comprises a series of parallel metal plates with rigid wires
 located between each two plates.  The plates are given an electrical
 charge  (i.e.,  either positive or negative), while the opposite charge  is
 imparted to  the wires.  The charged wires produce coronas which charge
 the fine fly ash particles with the opposite charge of the plates.  This
 causes  the particles to adhere to the oppositely charged plates.  The
 charges  alternate between the wires and the plates, subsequently removing
 more particles.  Each hour, the plates are rapped, and the adhering
 particles drop into a collection chamber where they are removed by a
 screw conveyor and carried to the quench water tank.
     The  fine fly ash fraction was collected from a sampling port in this
 screw conveyor.  The sample increments were collected by removing the
 port cover and allowing the port to bleed for approximately one minute.
 Then, a one pint sample was collected using a shovel.   This sampling
 method was analogous to the full-stream cut method used for sampling the
 coarse fly ash at the chute discharge.  After the sample was obtained, it
 was placed in the compositing bucket, and the bucket was covered with
 polyethylene sheeting.
     At the end of the compositing period, the material in the bucket was
 homogenized by pouring the material into a polyethylene bag and mixing.
Then, the homogeneous material was placed into the clean sample
containers, labeled,  and documented on chain-of-custody forms.  For the
fly ash samples,  an additional sample container was filled with 1/2 pint
of the material to obtain a fly ash composite sample for laboratory
 leachate testing.   Therefore,  this sample represented the four shifts  of
operation during which sampling was conducted.
     The four fly ash composite samples and the fly ash laboratory
 leachate samples  were collected during the second shifts on September  28,
and 29,  1986, and the first and second shifts on September 30, 1986.   Per
                                   3-40

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 sampling plan requirements, one of these samples (i.e., second shift on
 September 23, 1986) was collected in duplicate for field and laboratory
 quality control.  Three additional grab samples were also collected to
 more adequately characterize the fly ash.  These were discrete coarse,
 medium, and fine fly ash samples which were collected using the
 procedures detailed above.  These three additional samples were collected
 during the second shift on September 29, 1986.  The containerized samples
 were packed on ice in Igloo-type coolers and shipped to the laboratory by
 priority air express.
     Quench water - The quench water samples were grab samples collected
 in the middle of the shift.  This being the case, they were not
 representative of the entire shift of operation, but of .only the instant
 in time at which they were collected.  Therefore, any time-dependent
 variability of the quench water contaminant concentrations has not been
 accounted for in these samples.
     These quench water samples were collected from the end of .a.settling
 tank in which the quench water was clarified.   As the quench water tank
overflowed,  the water and associated debris spilled into this settling
 tank.   In the settling tank, the debris settled to the bottom, where it
was returned to the quench water tank via a drag conveyor.  At the end of
 the settling tank,  the clarified quench water overflowed a weir into a
 sump.   The water in the sump is pumped to the local POTW,  where it is
 treated and discharged.
     The quench water grab samples were collected at the overflow weir to
the sump.   A stainless steel dipper was used to collect an aliquot of the
overflowing material.   The dipper was passed through the overflowing
stream, at a constant speed, and was not allowed to overflow.  This
ensured that the grab sample was representative of the entire stream and
was not biased.   Next,  the water was poured into clean sample containers
 (i.e.  1-liter,  amber-glass bottles with teflon- lined screw caps), and
the appropriate  preservative was added (i.e.,  nitric acid for metal
                                   3-41

-------
samples and sulfuric acid for total organic carbon and organic scan
samples).  Then, the samples were labeled and documented on chain-of-
custody forms.  Finally, the samples were placed in Igloo-type coolers
and iced to maintain the chemical and physical integrity of the samples
during transport to the laboratory.  These quench water samples were
collected during the second shift on September 28, 1986, and during the
first shift on September 30, 1936.
     Production well ground water - During this first sampling visit, the
Versar monitoring team was unable to collect ground water samples from
the facility's monitoring wells.   A grab sample was collected from the
facility's production well on September 30, 1986, during the second shift.
     This ground water grab sample was collected from a tap at the
facility.  First, the tap was fully opened and allowed to discharge for
approximately two minutes to release any trapped sediments or gases.
With the tap still fully opened,  the amber-glass sample containers were
filled.   Then, the samples were labeled and documented on chain-of-custody
forms, and the appropriate preservative, either nitric or sulfuric acid,
was added.   Finally, the samples  were packed in a cooler and iced for
shipment to the laboratory.
     Landfill perimeter composite (disposed ash) - This sample was
collected on September 29, 1986,  to characterize the effects of
weathering on the disposed ash material.  The sample was a spatial
composite collected from the perimeter of the landfill and was designed
to adequately represent the wide  variety of disposed material.  Because
the landfill has been in use since  1970, the individual sample increments
represented a mixture of freshly  disposed material as well as older and
more weathered waste residue.
     The composite sample was collected using a hand-held auger to obtain
two-foot core sections.  The composite comprised 50 of these individual
increments.   The distance between sample increments was visually estimated
to yield 50 sampling locations around the landfill's perimeter.  Each
                                   3-42

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 increment was  collected by drilling  down  two  feet,  removing the  auger
 from the hole,  and placing the  sample core  in a compositing bucket.
 After the 50 increments were  collected, the material  in the bucket was
 mixed by stirring  with  a steel  garden trowel.  Then,  the sample  was
 containerized,  labeled,  documented,  and packed for  shipment to the
 laboratory.
      Blanks - Field blank and trip blank  samples were prepared to ensure
 that  the cleaning  water,  sample containers, and preservatives were not
 sources  of sample  contamination.  The blank samples were high purity
 HPLC-grade water poured into  the appropriate  containers with the required
 preservatives added.  This HPLC-grade water was used for field cleaning
 of sampling equipment.   The trip blank samples were prepared at Versar,
 and the  appropriate preservatives were added  to each sample.  A trip
 blank was prepared  for  each analyte  of interest and was carried to the
 facility during sampling  activities.  The field blank was prepared for
 total organic carbon and  was prepared while at the facility.
     Ground-water monitoring wella -  Facility C had three monitoring
 wells that were sampled  (3, 4,  and 17).   All  three of these wells were
 located hydraulically down-gradient of the disposal area between the
 landfill and a river.   Each monitoring well was equipped with a dedicated
 compressed-air pump that was used for evacuation and sampling.
     Prior to sampling the ground water,  the depth from the top of the
 well casing to the water surface was measured and recorded.  Then, the
 depth from the  top of the well casing to the sediment/water interface was
 measured and recorded.   The difference between these two measurements
 yielded the height of standing water in the well.   This height was used
 to determine the volume  of standing water in the well casing and saturated
annulus.   A volume of  water equal  to five times this standing water
volume was pumped from the well  to ensure that all water which had been
 in prolonged contact with the  well casing or the air was removed.
     After the  well evacuation was completed,  a grab sample was obtained
for pH and conductivity  analyses.   Then,  the ground water samples for
                                   3-43

-------
  chemical analysis were collected and placed directly into precleaned
  sample containers from the Teflon tubing that was attached to the pump.
  Because the water was clear without any visible particulate matter,
  filtering of the samples was not required.  After being collected, the
  samples were labeled, documented on chain-of-custody forms, packed in an
  Igloo-type cooler with ice, and shipped to the laboratory by priority air
  express.
       Field leachate Three field leachate samples were collected during
  the follow-up visit to Facility C.   These field leachates were grab
  samples collected from the north side and the northeast and northwest
  corners of the landfill.   The northwest corner sample was collected from
  an area where a natural leachate seep enters a small stream that flows
  underneath the landfill (i.e., through a culvert).  The other two samples
  (i.e.,  the north side and the northeast corner) were collected from
  surface water runoff streams along  the bottom edge of the landfill.
       All  three field leachate samples were collected using a borosilicate
  glass beaker to dip the sample and  pour it into the appropriate,
  precleaned sample containers.   At the northwest corner, sufficient
  standing  water was available to collect the sample without disturbing the
  sediment.   However,  as previously described in the introduction to this
  section,  the runoff streams at the  north side and northeast corner were
  too shallow to collect a  representative sample without disturbing the
  sediment.   Therefore,  the Versar monitoring tea.it used a shovel to dig a
  sample  collection basin in the runoff stream flow channel.  Before the
  samples were collected,  the runoff  stream was allowed to fill the basin,
  and the sediment was allowed to settle out of the collected leachate.
  After the  leachate had filled the basin and was allowed to clarify, the
  samples were collected by using the borosilicate glass beaker to dip the
  sample  from the collection basin.
       After all the samples were collected and containerized, they were
  labeled and documented on chain-of-custody forms.  Then, they were packed
  in coolers,  iced,  and shipped to the laboratory by priority air express.
                                     3-44
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-------
     3.3.4  Facility D
     Versar's monitoring personnel collected MWC residue samples, at
Facility D between October 2, 1986, and October 4, 1986.  These samples
included:  bottom/fly ash (i.e., a mixture of bottom ash and fly ash),
fly ash (i.e., a mixture of economizer ash and electrostatic precipitator
ash), quench water, disposed ash (i.e., a landfill perimeter composite),
and field leachate.  Per sampling plan requirements, 25 percent of these
samples were collected in duplicate for quality control purposes.  The
Versar monitoring team was unable to collect ground water samples because
Facility D did not have any functional monitoring wells.
     The MWC residue sampling at Facility D commenced during the first
shift on October 2, 1986, and was completed at the end of the second
shift on October 4, 1986.  During these sampling activities, both Unit
and Unit 2 were operating; however, because of the limited availability
of sampling locations, the individual units could not be sampled
separately.   Therefore, the MWC residue samples were representative of
both units operating in combination.   While the' samples were being
collected, the incinerator operator recorded pertinent operating data to
be used for evaluating contaminant concentration differences between
shifts and facilities (see Section 5.0).   This operating data is
presented in Section 4.1, Table 4.4.   Table 3.7 presents a summary,
including field sample numbers, of the samples collected at Facility D.
Detailed descriptions of the sampling locations and procedures for each
of the sample matricies are presented below.
     Bottom/fly ash - The Versar monitoring team had to collect a
combined ash (i.e., bottom and fly ash mixture) sample at Facility D
because a discrete bottom ash sampling location was not available.  The
bottom/fly ash sample included all the ash types generated by the
facility (i.e.,  bottom ash,  economizer ash, and electrostatic
precipitator ash).   These bottom/fly ash samples were time composites
representing one shift of operation and the average of both combustion
                                   3-45

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                                  TABLE 3.7  SAMPLE IDENTIFICATION COOES FOR FACILITY 0
  Sample
  Matrix

  Blank
  3 lank

Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
      Sample
    Description

    Field Blank
    Trip Blank

     Composite
Unit 1-2. 10/3. AM
Unit 1-2. 10/3. PM
Unit 1-2. 10/4, AM
Bottom/Fly Unit 1-2. 10/4. AM. Oup
Bottom/Fly   Unit 1-2. 10/4. PM

   Fly            Composite
   Fly         Composite, Oup
   Fly       Unit 1-2. 10/3. AM
   Fly     Unit 1-2, 10/3, AM, Oup
   Fly       Unit 1-2, 10/3, PM
   Fly       Unit 1-2. 10/4. AM
  -Fly       Unit 1-2, 10/4, PM

 Landfill    Perimeter Composite

 Leachate  •   Northeast Corner
 Leachate   Northeast Corner, Oup
 Leacnate     Southeast Corner
TOC
No.

19713
19725
Organic                                     PCOO/
 Scan    Metals      SNA         PCS         PCOF
  No.      No.       No.         No.         NO.
  19722    19726   19714-17    19724-25    19718-21
                        19639
                        19627
                        19614
         19625
         19612
                  19675
                  19682
                  19688
                  19691
                  19709
           19667
           19670
           19679
           19635
           19706

           19599

           19638   19628-31
           19626   19615-18
           19613   19602-05
                                   19677
                                   19684
                                   19690
                                   19693
                                   19712
    19600

19636-37
19623-24
19610-11
                         Lab
                      Leachate
                         No.
                                                               19678
                19676
                19683
                19689
               19692*
                19711


19669
19672
19681
19687
19708


19668
19671
19680
19686
19707
19673
19674





    19601

19632-35
19619-22
19606-09
  Quench        Unit 2, 10/3         19651    19648
  Quench      Unit 2, 10/3, Oup      19664
  Quench        Unit 2. 10/4         19704    19702
                                          19652   19640-43
                                          19665   19653-56
                                          1970S   19694-97
                                      19649-50
                                      19662-63
                                      19703.27
                                           19644-47
                                           19657-60
                                           19698-01
                   LEGEND:
                                  Bottoa/Fly - Conblned bottom ash and fly ash samples
                                  Fly - Fly ash
                                  MWell • GroundlMter from monitoring well
                                  Quench « Incinerator quench water
                                  TOC - Total organic carbon
                                  SNA • Base/neutral acid axtractable organics
                                  • • Sample collected but not analyzed
                                                  3-46

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units  (i.e.. Unit 1 and Unit 2).  The discrete grab sample increments
used to prepare the composite were collected every 40 minutes for a
six-hour period.
     At Facility D, bottom and fly ash were discharged into and collected
in two quench water tanks, one for each combustion unit.  After being
quenched, the ash material was subsequently discharged onto a belt
conveyor and transported to a load-out hopper, where it was loaded into a
truck for haulage to the landfill.  Due to the nature of the operation,
the belt conveyor could not be stopped to collect unit-specific bottom/
fly ash samples.  Therefore, the samples had to be collected at the load-
out hopper where the ash from each unit was mixed.
     The sample increments were collected as the load-out hopper
discharged into the truck.  A shovel was used to collect a full-stream
cut (ASTM Method 02234-76) of the ash material as it fell into the
truck.   The shovel was moved through the falling material at a uniform
rate to collect a representative portion of the falling stream.  This
sample portion was placed in a three-gallon bucket, which was covered
with polyethylene sheeting to prevent contamination during the
compositing period.
     At the end of the compositing period, the material in the bucket was
poured into a polyethylene bag and thoroughly mixed by inverting the bag
several times.   Before the sample was containerized, large pieces of
uncombusted material were removed to prevent sample bias.  Then, the
homogeneous material was placed into clean sample containers (i.e., one
glass wide-mouth quart jar for each PCDD/PCDF, PCB, and metals sample)
using a small steel garden trowel, and the samples were labelled and
documented on chain-of-custody forms.  An additional wide-mouth jar was
filled 1/4 of the way to obtain the bottom/fly ash composite sample for
laboratory leachate testing.  This laboratory leachate composite sample
was prepared in such a way that it was representative of the four shifts
of operation during which sampling was performed.
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     Th« four bottom/fly ash composite samples and the one bottom/fly ash
 laboratory leachata composite were collected during the first and second
 shifts on October 3 and 4, 1986.  Additionally, per sampling plan require-
 ments, one of these samples (i.e., first shift on October 4, 1986) was
 collected in duplicate for field and laboratory quality control.  The
 containerized samples were placed in Igloo-type coolers with ice and
 carried to the laboratory by the Versar monitoring team.
     Fly ash - Similar to the bottom/fly ash samples, the fly ash samples
 were time composites representing one shift of operation and the average
 of the two combustion units.   Also like the bottom/fly ash samples, the
 fly ash samples were collected every 40 minutes over a six-hour period.
 However, unlike the bottom/fly ash samples, the fly ash sample increments
 had to be collected from each combustion unit individually.  Consequently,
 because the operating capacities of the units were similar, equal volumes
 of fly ash were collected from each unit and manually composited.
     Facility D generated two different fly ash fractions—coarse fly ash
 and fine fly ash.  The coarse fly ash fraction is removed from the flue
 gas stream in an economizer.   The economizer is simply a series of bends
 that decrease the flue gas velocity causing the coarse particles to
 settle out of the stream and fall down a chute to the quench water tank.
 The fine fly ash fraction is removed from the flue gas by a series of
 electrically charged parallel plates in the electrostatic precipitator
 (ESP).   The fine ash particles have a static charge which causes them to
 be attracted to the oppositely charged plates.  The charges on the plates
are alternately changed from positive to negative, subsequently removing
more of the oppositely charged particles.  Each hour, the plates are
 rapped, and the adhering fine ash particles fall into a screw conveyor
which carries the material to the chute where it joins the economizer
 ash.  The fly ash sample increments were collected from sampling ports  in
 this chute.
     The sample increments were collected by using a stainless steel
 dipper to obtain a full-stream cut of the falling material.  The sampling
                                   3-48

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 port cover was removed,  and the dipper was  inserted perpendicular to the
 falling stream.   Because the dipper opening cross-sectional  area  was
 approximately equal to the  interior cross-  sectional area  of the  chute,
 it was ideal for collecting a representative unbiased cut.   The dipper
 was held in the  part and allowed to fill  without  overflowing.  Then, the
 sample increment was placed in a compositing bucket,  and the bucket was
 covered with polyethylene sheeting.  This procedure was  repeated  for each
 unit collecting  equal sample portions  (i.e.,  one  full dipper)  from each.
      At the end  of  the compositing  period,  the material  in the bucket was
 homogenized by pouring the  material  into  a  polyethylene  bag  and mixing.
 Then,  the  homogeneous material  was  placed into precleaned  sample
 containers,  which were labeled  and  documented on  chain-of-custody forms.
 Two additional 1-quart sample containers  were partially  filled with
 1/2 pint of each shift composite  fly ash  to obtain  duplicate fly  ash
 composite  samples,  for laboratory leachate  testing.   Therefore, these two
 samples represented the  four shifts  of operation  during  which  sampling
 was  conducted. .
     The four fly ash composite samples.and the two fly  ash  laboratory
 leachate samples  were  collected during the  first  and  seconds shifts on
 October 3 and 4,  1986.   Per sampling plan requirements,  one of these
 samples (i.e., first  shift on October 3,  1986) was  collected in duplicate
 for  field and laboratory quality control.    The containerized samples wers
 placed in Igloo-type coolers with and carried to  the  laboratory by the
 Versar monitoring team.
     Quench water - The quench water samples were grab samples collected
 in the middle of the first shifts on October  3 and  4, 1986.  Consequently,
 they were not representative of the entire  shift of operation, but of
only the instant in time at  which they were collected.   Therefore,  any
time-dependent variability of the quench water contaminant concentrations
has not been accounted for by these samples.
                                   3-49

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      The  quench water samples were collected from the end of the quench
 water tank using a stainless steel dipper.  Unlike the bottom/fly and fly
 ash samples  that were representative of both combustion units, the quench
 water samples were representative of only Unit 2 because an adequate
 (based on safety considerations) sampling location was not available for
 Unit 1.   The samples were collected by placing the dipper in the quench
 water tank and allowing it  to fill.  Then, the collected sample was
 split equally among the required number of pracleaned sample containers
 (i.e., eleven 1-liter amber-glass bottlas and one 4-ounce TOC bottle per
 sample).  On October 3, 1986, a duplicate sample was collected by
 splitting each dipper among two complete sets of glass containers.  The
 reason for splitting each filled dipper among the required containers was
 to prevent sample bias arising from each discrete grab.   This procedure
 was  repeated until all of the sample .bottles were full.
     After the sampling was completed, the appropriate preservative (i.e.,
 nitric acid for metal samples and sulfuric acid for total organic carbon
 and. organic scan samples) was added to each sample, and the containers
 were  securely capped.  Then, the samples were labeled and documented on
 chain-of-custody forms.   Finally, the samples were placed in Igloo-type
 coolers and iced to maintain the physical and chemical integrity of the
 samples during transport to the laboratory.
     Landfill perimeter composite (disposed ash)  - This  sample was
 collected October 2,  1986, to characterize the effects of weathering on
 the disposed ash material.  The sample was a spatial composite collected
 from the perimeter of the landfill designed to adequately represent the
wide variety of disposed material.   Because the landfill has been in
continuous use for several years, the individual  sample  increments
 represented a mixture of freshly disposed material as well as older and
more weathered waste  residue
     The composite sample was collected using a hand-held auger to obtain
 two-foot core sections.   The composite comprised 50 of these individual
                                   3-50

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 sections.   The  distance  between sample  increments was visually estimated
 to yield 50 sampling  locations around the  landfill's perimeter.  Each
 increment  was collected  by drilling down two feet into the material,
 removing the auger  from  the hole, and placing the sample core in a
 compositing bucket.   After the 50 increments were collected, the material
 was mixed  by vigorously  stirring with a steel garden trowel.  Then, the
 sample was  containerized, labeled, documented, and packed on ice for
 shipment to the  laboratory.
     Field  leachate - Three field leachate samples were collected at
 Facility 0  on October 2, 1986.  Facility 0 has a leachate collection
 system installed for  the landfill, however, the system was obstructed, so
 no leachate  could be  obtained.  Leachate samples were collected from
 natural depressions where surface water runoff and natural seeps
 collected along  the bottom of the landfill.  The field leachates were
 grab samples collected from two of these depressions at the southeast and
 northeast corners of  the landfill.  The sample from the northeast corner
 was collected in duplicate for quality control purposes.
     All three field  leachate samples were collected using a stainless
 steel dipper.  The dipper was placed in the depression and allowed to
 fill with leachate.  Then, the sample increment was split equally among
 the required number of precleaned sample containers (i.e., eleven 1-liter
 amber-glass bottles and one 4-ounce TOG bottle for the southeast corner,
 and twice as many containers for the duplicate samples at the northeast
 corner) to prevent sampling bias.   This procedure was repeated until all
 of the samples bottles were full.   The sample containers were securely
 capped, labeled, and documented on chain-of-custody forms.  Finally, the
 samples were placed in coolers, iced, and personally delivered to
Versar's laboratory by the field team.
     Blanks - Field and trip blanks were prepared to ensure that the
cleaning water,  sample containers, and preservatives were not sources of
sample contamination.   The blank samples were high purity HPLC-grade
                                   3-51

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 water/  which was used for field cleaning of sampling equipment, poured
 into  the  sample containers with the appropriate preservatives added.  The
 trip  blanks were prepared at Versar and were carried to the facility
 during  sampling activities.  The field blank was prepared for total
 organic carbon, while at the facility.
      3.4  Sample Preparation and Analysis Procedures
      The  solid residue samples (e.g., fly ash, bottom ash, and disposed
 ash)  and  the liquid samples (e.g., field leachate, ground water, and
 quench  water) that were collected from the specified facilities using the
 procedures detailed in Sections 3.3.1 through 3.3.4 were analyzed to
 determine the concentrations of various toxic metals and organic
 compounds.  The solid samples were prepared for metal analyses using
 SW-846  Method 3050 (i.e., acid digestion) and for PCB analysis using
 modified SW-846 Method 3540 (i.e., soxhlet extraction) with a 1:1 mixture
 of hexane and acetone as the extraction solvent.  The solid samples for
 PCDD/PCDF analyses were prepared according to the protocols specified in
 the analytical method (see Appendix B).  For analytical QA purposes,
 25 percent of the samples were collected in duplicate and submitted to
 the laboratory as "blind" field duplicates.   Blanks, laboratory
 duplicates,  spiked samples, and check standards were analyzed according
 to specification in the procedure and at a minimum frequency of 5 percent.
     In addition to these solid and liquid samples, leachates were
prepared in the laboratory from the solid residue samples and analyzed
for metals and organics.   The laboratory leachates were prepared from
composites of the solid samples (i.e., one fly ash and one bottom ash
composite per facility)  by using three different extraction techniques:
Extraction Procedure (EP),  Toxicity Characteristics Leaching Procedure
 (TCLP),  and Mono-filled Waste Extraction Procedure (MWEP; SW-924).  These
 leaching procedures and the analytical methods are described in the
following sections.
                                   3-52

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     3.4.1  Laboratory Leachates
     The laboratory leachate composite samples from each facility were
 subjected to three different leaching procedures in attempt to compare
 the data resulting from the use of three commonly accepted extraction
 methods.  These leaching procedures were developed in order to
 standardize the extraction procedure used and to approximate natural
 leaching potential in the absence of field leachate composition data by
 determining the type and quantity of leachable chemical constituents
 within a solid waste.  The leaching characteristics of the wastes are
 essential input data for designing landfills and leachate treatment
 facilities.  Additionally, the EP and TCLP methods have regulatory
 significance; the leaching characteristics from these methods are used to
 classify a solid waste as hazardous or non-hazardous under the Resource
 Conservation and Recovery Act (RCRA).  Conversely, the MWEP method was
 developed only to provide leaching characteristic information and has no
 regulatory significance.  A summary of the conditions for these leaching
 procedures is provided in Table 3.3.   A brief description of each
 leaching procedure is presented below.
     Extraction Procedure (EP) - This laboratory leaching procedure was
 applied to composite samples of fly ash and bottom (or bottom/fly) ash
 from each facility.   Since this procedure was developed to classify a
 solid waste as hazardous or non-hazardous based on predetermined hazard
 levels for 14 specific constituents,  the analytical results from these
 EP-prepared residues may be used to formulate regulatory strategies and
 to evaluate the adequacy of current disposal practices.  Therefore, the
EP test procedure was followed very closely.  Assuming the collected
 solid residue sample contained no filterable liquid (i.e., it contained
only surface and interstitial moisture), the EP method was performed as
 follows:
     1.  Obtain a representative 100-gram sample of residue.
     2.  Crush material  to <9.5 mm, if necessary.
                                   3-53

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                   Table  3.3.   Suamry Conditions for EP, TO.P,  and HHEP Methods
Conditions
Liquid.-Solid Ratio
Extraction Medium
pH Control
Extraction Tim
Agitation Method
Temperature Control
Particle Size
Hunter of Extractions
EP (1)
20:1
0.5N acetic acid
5
24 hours
Tuabler
20-40 C
< 9.5 itn
1
Tap (2)
20:1
0.1N acetate buffer
5
18 hours
Tunbler 9 28-32 rpa
19-25 C
< 9.5 im
1
MNEP (3)
10:1 per extraction
Distil led/delonlzed water
None
18 hours per extraction
Tunbler
24-26 C
< 9.5 ma
4. sequentially (4)
(1)  EP - Extraction Procedure (40 CFR 261. Appendix II).
(2)  TCLP - Toxldty Characteristic Leaching Procedure (Revised 40 CFR 261.  Appendix II).
(3)  MMEP - Motion lied Haste Extraction Procedure (A Procedure for Estimating Monofllled Solid
      waste Leachate Composition, Technical Resource Document SW-924, 2nd Edition).
(4)  For this project, a modified MHCP method was used with two sequential extractions
                                                3-54

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     3.  Place sized solid residua in extractor vassal.
     4.  Add amount of daionized water equal to 16 times the weight of
         the solid residue.
     5.  Begin agitation and measure pH.
         5a.  If pH >5.0. adjust to 5.0 ± 0.2 with 0.5N acetic acid.
         5b.  If pH <5.0, no adjustment is necessary.
     6.  Continue monitoring pH at specified intervals adjusting pH as
         required in 5a for 6 hours.
     7.  Agitate mixture for a total of 24 hours between 20-40°C.
         7a.  If at the end of 24 hours the pH > 5.2, adjust to 5.0 ±
              0.2 and continue agitation for an additional 4 hours.
         7b.  If pH <5.2, no additional agitation is necessary.
     8.  Add required amount of daionized water and filter mixture using
         a 0.45 m membrane filter.
     9.  Analyze or preserve filtrate (i.e., laboratory leachate) as
         required.
     If the residue sample contained filterable liquid, the sample was
first separated into its component phases (i.e., the sample was
filtered),  and the above procedure was carried out on the solid phase.
Then, the initial filtrate and extract from the solid phase were combined
for analysis.   Finally, the EP leachate was analyzed for metals, total
organics (i.e.,  organic scan), and if the IOC results from the MWEP
extract exceeded 5 mg/L, organic constituents (i.e., BNA's).  As
specified in the sampling plan, 25 percent of these samples were
collected,  prepared,  and analyzed in duplicate as blind (i.e., to the
analysts) QA/QC samples.
     Toxicity Characteristic Leaching Procedure (TCLP) - Like the EP
method, this laboratory leaching procedure was applied to composite
samples of  fly ash and bottom (or bottom/fly) ash from each facility.
The TCLP method was developed to replace EP as the hazardous waste
classification criteria under RCRA.   The TCLP classification criteria are
based on all Appendix VIII (40 CFR 261) constituents, including volatiles,
while EP classifications are based on predetermined hazard levels for only
                                   3-55

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 14 spacific contaminants.  Therefore, the analytical results from the

 TCLP-prepared extracts nay be more likely to be applied to a broader

 range of waste types than those from the EP-prepared extracts.  Assuming

 that the solid residue sample contained no filterable liquid, the TCLP

 method was performed as follows:

     1.  Obtain a representative 100-gram sample of residue.

     2.  Crush material to <9.5 mm, if necessary, and place residue in
         extraction vessel.

     3.  Determine appropriate extraction medium:
         3a.   Weigh out 5-gram subsample of residue; reduce particle size
              to <1 mm, if required;  place sample in a 500 ml beaker.
         3b.   Add 96.5 ml of distilled/deionized water (ASTM Type II).
         3c.   Stir sample vigorously for 5 minutes with magnetic stirrer.
         3d.   Measure pH, and if pH <5 use Extraction Fluid 1.
         3e.   If pH >5, add 3.5 ml iTON HC1;  slurry for 30 seconds;  heat
              to 50°C for 10 minutes.
         3f.   Allow mixture to cool to room temperature and measure pH.
         3g.   If pH <5, use Extraction Fluid 1, and if pH >5, use
              Extraction Fluid 2.

     4.  Add amount of extraction fluid selected in Step 3 equal to
         20 times the weight of the solid residue.

     5.  Close extraction vessel,  and agitate in rotary extractor device
         at 30 •»• 2 rpm for 13 hours,  maintaining the temperature at
         22 ± 3"C.

     6.  Filter material through a 0.6 to 0.3 urn glass fiber filter.

     7.  Analyze or preserve filtrate as required.

     If the residue sample contained filterable liquid, the sample was
first separated into its component phases, and the above procedure was
carried out on the solid phase.  Then, if the initial filtrate and solid

extract were  compatible (i.e., did not form multiple phases or precipi-

tates upon combination), they were combined together for analysis.  If

these liquids were incompatible, they were analyzed separately, and the

results were  mathematically combined to yield the total leachable

composition of the solid residue sample.  Finally, the TCLP leachate was
                                   3-56

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 analyzed for metals, total organic3 (i.e., organic scan), and BNA's (i.e.,
 if the IOC results from the MWEP extract exceeded 5 mg/L).  Although not
 specified in the scope of work, the TCLP leachates were also analyzed for
 PCOO/PCDF at the request of EPA/OSW to determine whether this method
 would extract these hazardous organic compounds.  As specified in the
 contract, 25 percent of these samples were collected, prepared, and
 analyzed in duplicate as blind QA/QC samples.
     Mono-filled Waste Extraction Procedure (MWEP) - As was the case for
 the EP and TCLP methods, this laboratory leaching procedure was applied
 to composite samples of fly ash and bottom (or bottom/fly) ash from each
 facility.  The MWEP method was developed to estimate the quantity of
 potentially leachable constituents in a given solid waste and to measure
 the concentration of these constituents in extracts produced by various
 solid to liquid extraction ratios.  This procedure includes a sequential
 four-step batch extraction which produces data that can be used to
 construct an aqueous extraction profile for each of the constituents.
 For this MWC residue study, however, Versar used a modified MWEP method
with only two sequential batch extractions.  Unlike the EP and TCLP
methods, the MWEP has no regulatory significance.  The justification for
 using this method is its applicability to mono-filled wastes only, which
 was one of the facility selection criteria (See Section 3.1.1).  The
 modified MWEP method was performed as follows:
     1.   Obtain subsample and determine percent solids.
     2.   Obtain representative sample equal to 100 grams dry weight and
         place in extraction vessel.
     3.   Add appropriate amount of distilled/deionized water to give a
         10:1 liquid to solid weight ratio, taking into account the
         moisture determined in step one.
     4.   Extract (i.e., agitate using a tumbler) the mixture for 13 hours
         at  a temperature of 25 ± 1°C.
     5.   Filter mixture through a 0.45  urn nitrocelluse membrane filter
         (for inorganic analyses) or a  0.6 - 0.3 urn glass fiber filter
         (for organic analyses).
                                   3-57

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      6.   Retain  filtrate  for subsequent analysis.  Place in properly
          cleaned sample container and preserve as required.
      7.   Place filter cake  (i.e., solid residue) back into extraction
          vessel  and add 1 liter of fresh distilled/deionized water.
      3.   Repeat  steps 4 through 6.
      9.   Analyze  the two sequential extracts separately.
      Each of the  two extracts ware analyzed for metals, total organics
 (i.e., organic scan), and total organic carbon (TOG).  If the TOG
 concentration of  either extract was greater than 5 mg/L, then the EP and
 TCLP  extracts, as well as both MWEP extracts, were analyzed for organic
 constituents (i.e., BNA's).  The EP and TCLP extracts were not analyzed
 for total organic carbon because an organic acid (i.e., acetic acid) was
 used  for  pH control during the leaching procedure.   As specified in the
 sampling  plan, 25 percent of these samples were collected, prepared, and
 analyzed  in duplicate as blind QA/QC samples to determine the
 reproducibility of sampling, preparation,  and analysis procedures,
      3.4.2  Analyses
     Analyses required by the Scope of Work included total organic
carbon, total metals (i.e.,  As, Cd,  Cr,  Cu, Pe, Hg,  Mn, Ni, Pb, Se, and
Zn), organic scan, PCQD/PCDF, and PCB's.   Additionally, the analysis of
organic constituents (i.e.,  BNA's) was required contingent upon the
 results of the total organic carbon and organic scan analyses.  All of
these analyses were conducted using EPA-approved procedures.   Table 3.9
provides the analytical methods, techniques, and detection limits for
these analyses.   It should be noted that although Table 3.9 gives the
primary analytical method reference (e.g.,  SW-346 and MCAWW), the methods
were applied as modified by the Contract Laboratory Program (CLP)
Statement of Work for the applicable analytes (i.e., metals and BNA's).
A brief description of the analytical methods used for each parameter is
presented below.
                                   3-58

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                           Table 3.9.   Sunery of Analytical Methods and Detection Halts
                                      Liquid Samples  (1)
Solid Samples (2)

Parameter
Total Organic Carbon
Organic Scan
Arsenic
Cadmium
Chromium
Copper
Iron
Lead
Manganese
Mercury
Nickel
Selenium
Zinc
PCOO/PCOF's
PCB's
Organic Constituents
Analytical
Method (3)
MCAWW-415.1
MCAMM18.1
MCAWM-206.2
MCAWW-200.7
MCAWW-200.7
MCAWW-200.7
MCAWN-200.7
MCAWW-239.2
MCAWM.200.7
MCAWW-245.1
MCAWM.200.7
MCAWH-270.2
MCAHW-200.7
Appendix B
Appendix C
ORG-625
Analytical
Technique (4)
COMB/OXIO
IR SPEC
Furnace AA
I CAP
I CAP
I CAP
I CAP
Furnace AA
I CAP
Cold Vapor AA
I CAP
Furnace AA
I CAP
HRGC/HRMS
HRGC/EIMS
6C/MS
Detection
Limit (5)
1 rag/L
0.25 ng/L
10 ug/L
5 ug/L
10 ug/L
25 ug/L
100 ug/L
5 ug/L
15 ug/L
0.2 ug/L
40 ug/L
5 ug/L
20 ug/L
20 ng/L
S-50 ug/L (6)
10-50 ug/L (7)
Analytical
Method (3)
N/A
N/A
SH846-7060
SW846-6010
SW846-6010
SW846-6010
SW846-M10
SW846-7421
SH846-6010
SW846-7471
SW846-6010
SW846-7740
SW846-6010
Appendix B
Appendix C
N/A
Analytical
Technique (4)
N/A
N/A
Furnace AA
I CAP
I CAP
I CAP
I CAP
Furnace AA
I CAP
Cold Vapor AA
I CAP
Furnace AA
I CAP
HRGC/HRMS
HRGC/EIMS
N/A
Detection
Limit (5)
N/A
N/A
1.0 mg/kg
0.5 rag/kg
1.0 mg/kg
2.5 ng/kg
10 mg/kg
0.5 ng/kg
1.5 mg/kg
0.02 mg/kg
4.0 mg/kg
0.5 ng/kg
2.0 mg/kg
20 ug/kg
0.2-1 ug/kg (6)
N/A
N/A - Not Applicable; these analyses will not be conducted on solid samples.
(1) - Liquid samples include:  field leachate. quench water, ground water, and laboratory leachate.
(2) - Solid samples include:  fly ash, bottom ash, disposed ash, etc.  Solid samples will be prepared for metals analyse?
        using SW-846 Method 3050—Acid Digestion.
(3) - Referenced analytical methods are fro* the primary sources listed below, however,  these methods will be applied
        as modified by Contract Laboratory Program (CLP) Statement of Work for metals and organic constituents.
      MCAHW - U.S. EPA, Methods for Chemical Analysis of Water and Wastes. March 1983 (EPA-600/4-79-020).
      ORG - U.S. EPA, Methods for Organic Chemical Analysis of Municipal and Industrial  Wastewater.  July 1982 (EPA-600/4-.a
      SW846 • U.S. EPA, Test Methods for Evaluating Solid Wastes - SW-846, April 1984.
      Appendix B • Analytical Procedures to Assay Stack Effluent Samples and Residual Combustion Products for
        Polychlorinated 01benzo-p<0toxins (PCDO) and Polycnlorinated Olbenzofurans (PCOF).  Group C - Environmental
        Standards workshop (ASME. U.S. DOE. and U.S. EPA), September 1984.
      Appendix C - Method 680.  Determination of Pesticides and PCBs in Water and Soil/Sediment by Gas Chromatography/Msss
        Spectrometry, U.S. EPA, EMSL. Cincinnati. OH, November 1985.
(4) - COMB/OXIO - Combustion/Oxidation; IR SPEC - Infrared SpectrophotometHc; I CAP - Inductively Coupled Argon
        Plasma; HRGC/HRMS - High Resolution Gas Chronatography (Capillary Column)/H1gh Resolution Mass Spectrometry
        HRGC/EIMS - High Resolution Gas Chrometography/Electron Impact Mass Spectrometry; GC/MS - Gas Chromatography/
        Mass Spectrometry.
(5) - Detection limits  are Contract Required Detection Limits (CRDLs) from CLP for metals and organic constituents.
(6) - Detection limits  increase with increasing level of chlorlnatlon.   Solid samples will  be prepared for PCB analyses
        using SW-846 Method 3540—Soxhlet Extraction.
(7) . Detection limits  for individual constituents are listed 1n the iwthod.

                                                          3-59

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      Total Organic  Carbon (TOC) - Total organic carbon analysis was
 performed on all  field water samples  (i.e.,  field  leachate, quench water,
 and ground water) and laboratory leachate prepared using MWEP.  The
 results  of the  total  organic carbon analyses were  used to initiate the
 BNA contingency analysis.  Each field water  sample that had a TOC con-
 centration of greater than 5 mg/L was analyzed for BNA's.  Additionally,
 if  either of the  two  MWEP extracts contained greater than 5 mg/L TOC,
 then the  EP,  TCLP,  and both MWEP extracts were analyzed for BNA's.
      The  TOC analysis was  performed by converting  the organic carbon in
 the  sample  to carbon  dioxide by catalytic combustion.  Then, the carbon
 dioxide was  measured  using infrared detection.  Prior to analyzing each
 batch of  samples, the infrared detector was calibrated by analyzing a
 blank and three standards, and plotting a curve of peak area (from a
 strip chart  recorder)  versus concentration.  Finally, the measured amount
 of carbon dioxide in  the sample (i.e., the peak area) was compared to the
 calibration  curve to  determine the TOC concentration of the sample.
      Organic  Scan - The organic scan was performed on all field water
 samples and  laboratory leachates to determine whether organic compounds
 other than PCDD's, PCDF's, and PCB's were present.   The organic scan was
 performed by  acidifying the sample to pH <2 and extracting it with
 fluorocarbon  113 in a  separatory funnel.   The extract was analyzed using
 an infrared spectrophotometer that was calibrated before each batch of
 samples using five calibration standards that bracketed the expected
 sample concentration.   The calibration curve was constructed by plotting
 the absorbence of these standards versus their respective concentrations,
and the organic content of the sample was determined by direct comparison
of its absorbence to the standards.
     Metals - Total  metal analyses were performed on all field water
 samples,  laboratory leachates,  and solid samples.   The solid samples and
 liquid samples containing particulate matter were prepared using EPA
Method 3050 (SW-846),  as modified by CLP,  which is an acid digestion
                                   3-60

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 procedure.  After the sample was digested,  it was analyzed using the
 appropriate technique:   Cold Vapor Atomic Absorption (Hg), Graphite
 Furnace Atomic Absorption (As,  Pb, and Se),  or Inductively Coupled Argon
 Plasma (Cd. Cr,  Cu,  Fe,  Mn,  Mi,  and Zn).
      The Cold Vapor  AA  technique is a flameless AA procedure  based on the
 absorption of radiation by mercury vapor.   First,  the  mercury was  reduced
 to the elemental state  and aerated from solution in a  closed  system.
 Then,  the mercury vapor  passed  through a cell positioned in the  light
 path of an AA spectrophotometer.   The spectrophotometer  was calibrated
 before each day  of analysis  using a blank and five mercury standards  to
 construct a calibration  curve of absorbence  versus micrograms of mercury.
 The absorbence of the sample (i.e.,  peak height on a strip-chart recorder)
 was compared to  the  calibration  curve to determine the mercury concentra-
 tion of the sample.
     The  Graphite Furnace  technique  also  used an AA spectrophotometer to
 determine  the  metal  concentration.   The  spectrophotometer  was calibrated
 daily  before analysis for  each metal  by using a blank  and  three  calibra-
 tion standards that  bracketed the  expected sample  concentration.   The
 standards were analyzed, and internal  curves  of absorbence versus
 concentration  were constructed by  a microcomputer.   This calibration
 procedure had  to  be  performed each time a new metal  was analyzed.
     For Graphite Furnace AA analysis, a  representative aliquot  of  the
 sample was  placed  in a graphite tube within the  furnace, evaporated to
 dryness, charred, and atomized.   Concurrently,  energy  (i.e.,  a beam of
 light at a wavelength specific to  the metal of  interest from  a hollow
 cathode tube) was directed through the graphite  tube containing  excited
 energy level atoms of the vaporized metal.  The  intensity  of  the trans-
 mitted radiation was used to determine the absorbence  (A =  2  - log  %  T),
which is directly proportional to  the concentration  of the  metal atoms
contained in the vapor.   This absorbence was measured, and  the specific
metal concentration was  determined by direct comparison to  standards
 (i.e.,  the internal calibration curve).
                                   3-61

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     Unlike the previous two methods, the ICAP procedure can be used to
measure the concentrations of several different metals, concurrently..
The previous two methods can only quantify one particular metal in each
sample aliquot, but they were used because they generally offer greater
sensitivity (i.e., a lower detection limit).
     Prior to analysis each day, the ICAP instrumentation was calibrated
for each metal analyte of interest by using two blanks (i.e., calibration
blank and a reagent blank) and three standards that bracketed the
anticipated sample concentrations.  Before analyzing these standards, the
analyst entered the actual standard concentrations for each metal into
the ICAP computer.  Subsequently, during the analysis of the calibration
standards, the computer generated initial calibration curves based on
these entered concentrations and the characteristic atomic-line spectra
intensities.
     During ICAP analysis, the sample was reduced to a fine spray (i.e.,
an aerosol) and transported to a plasma torch where excitation occurred.
Then, characteristic atomic-line spectra were produced for each metal
present in the aspirated sample, and these spectra were dispersed by a
grating spectrometer.   Finally, the intensities of the dispersed metal
characteristic spectral lines were compared to standards (i.e., the
internal calibration curves) to yield the concentration of each metal in
the sample.
     PCDD/PCDF - PCDD/PCDF analyses were performed on all fly ash
samples.  When the results of these analyses showed concentrations of
total PCDD's  or PCDF's in any of the four fly ash samples from a given
facility exceeding 5 ng/g, the bottom (or bottom/fly) ash samples,
TCLP-prepared leachates, field leachate samples, and quench water samples
from that facility were analyzed for PCDD/PCDF.  The analytical method is
designed to quantify the individual homologs (homolog refers to the total
number of chlorine atoms in the organic structure, but not to the
position of those atoms) in the tetra- through octa-chlorinated classes/
                                   3-62

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 but not  to quantify the  individual  isomers within these classes.  One
 notable  exception was the 2,3,7,3-TCDD  isomer, which was quantified.  The
 PCDO/PCDF analyses were  performed by Versar's subcontractor. Battalia
 Columbus Laboratories.   The analytical  method used by Battalia  is
 included in this report  as Appendix B.
     The first step of this analytical  method was a sample extraction
 procedure using the appropriate organic solvent(s).  Next, the  extract
 was  subjected to a sequence of liquid chromatography elutions to remove
 co-extracted interferences.  Then, the  cleaned extract was introduced
 into a capillary column  gas chromatography instrument with a high
 resolution mass spectrophotometer for identification and quantification
 of the individual constituents.  Prior  to analyzing for PCDD/PCDF, the
 GC/MS system was calibrated using three standards that bracketed the
 expected sample concentration range.  Finally, the homologs were
 identified and quantified by comparison of their retention times and mass
 spectral intensity ratios to those of the calibration standards.
     PCB's - Analysis of PCB's was performed on all fly ash samples.  If
 the  results of the PCDD/PCDF analyses triggered the analysis of bottom
 (or bottom/fly) ash samples, field leachates, and quench water samples
 from a given facility as discussed above, the contingency analyses for
 PCB's were also performed on these samples.  Similar to the PCDD/PCDF
 analytical method,  the PCB method was used to identify and quantify the
 PCS homologs,  and not the individual isomers.
     All field water samples were analyzed by EPA Method 630 subtitled
 "Determination of Pesticides and PCBs in Water and Soil/Sediment by Gas
Chromatography/Mass Spectrometry."  The analytical method is incorporated
 into this report as Appendix C.
     This method was recommended by Ms. Ann Alford-Stevens of EPA Environ-
mental Monitoring and Support Laboratory (EMSL) in Cincinnati, Ohio.
Method 630 is  a published,  validated method for water samples only.  It
 is the most  current GC/MS analytical procedure for the determination of
                                   3-63

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PCBs identified and measured as isomer groups or horoologs.   Also
developed with the method is a software package which automates the data
reduction to the full-scan GC/MS data generated by the method.
     EPA Method 680 does not provide a procedure for extraction of PCBs
from solid samples, however.  The Versar laboratory tested and adapted
SW-346 Method 3540, a general extraction procedure, to the extraction of
PCBs from fly ash and combined bottom/fly ash samples.  Preliminary tests
were conducted using the 20 fly ash samples from the four facilities to
verify that the extraction procedure was valid.  These tests and the
results are described below.
     •  Method Tests
     The method tests consisted of two trial runs of the method using a
blank, a standard, and a real ash sample.  The combined methods to be
tested included the following steps:
     1.  Soxhlet extraction of the fly ash with acetone/hexane
     2.  Acid cleanup of the extract
     3.  Micro florisil column cleanup of the extract
     4.  Full scan GC/MS analysis of the samples
     5.  Data reduction using the automated software for Method 680
     For the first test, the test "samples" were processed through all of
the steps listed above.  The results indicated a serious problem with the
method.  No surrogates were recovered.  The problem was determined to be
in the extraction process.  Overall there did not seem to be any major
problems with applying the analytical procedures to the samples, but the
problem with surrogate recovery had to be resolved.
     A second test was initiated.  For the second test, the cleanup
procedures, which were suspected to be the problem, were omitted.  The
surrogates were recovered.  The analysis showed that  the second test was
an improvement over the first but that there were still some problems.
Additional tests showed that there were  losses occurring during the
                                   3-64

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concentration step of the final extract.  After rinsing the walls of the
concentration vessel, the recoveries were much better.
     After the second test is was decided to proceed with samples without
the cleanup.  The cleanup was suspected of contributing to the recovery
deficiency/ and the samples analyzed did not present an analytical
problem without the cleanup.
     •  Fly Ash Extraction Method 3540 Summary
     Samples were extracted using SW-846 Method 3540 adapted to ash
samples.  Twenty grams of the ash samples were weighed out.  Each sample
aliquot was spiked with stable labeled PCS surrogates (carbon
4-chlorobiphenyl, carbon   3,3'-4,4'-tetrachlorobiphenyl, carbon
2,2',3,3',5,5',6,6'-octachlorobiphenyl, and carbon   decachloro-
biphenyl).  Soxhlet extraction with 1:1 acetone/hexane was performed for
16 hours.
     The extract was then concentrated to a final volume of 50 ul for
analysis.  The following changes were made to the method:  sample size
was increased to 20 grams, no sodium sulfate was added to the sample
during extraction, and the final volume was adjusted to 50 ul.
     •  Fly Ash Analysis Method 680 Summary
     Samples were analyzed using U.S. EPA Method 630.  Four surrogates
were added to samples prior to extraction, and one internal standard was
added to each extract before GC/MS analysis.  The analysis was performed
on a Finnigan 5100 GC/MS DS.   The chromatographic column used was a Restek
RTX-5 30-meter 0.32 mra-id fused silica capillary column temperature
programmed from 80C to 302C at 15C per minute.  Samples were injected in
the splitless mode.  The scan range was 45-550 amu.
     Prior to analysis,  the system was calibrated to FC-43 and adjusted
to meet U.S.  EPA calibration requirements for 10 ng of DFTPP.  An initial
five point calibration curve was generated by injecting 1 ul aliguots of
calibration standards supplied by EMSL Cincinnati.  The calibration curve
                                   3-65

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was checked daily with a continuing calibration check standard before
each  12-hour sequence..
      PCBs were identified and measured by isoraer group (homolog).  The
automated software utilizes characteristic mass spectral features of PCBs
at each level of chlorination for identification.  Additional mass spectral
confirmation checks were made by chemists after the automatic selection
and quantification of PCBs was completed.  Adjustments to the PCS
concentration were made in those instances where additional professional
mass spectral interpretation disagreed with the confirmation made by the
automated data reduction program.  The additional checks consisted of
verifying acceptable quantitation and confirmation ion ratios, presence of
M-70 confirmation ion, and absence of M+70 and M+35 interfering ions.
     •  Detection Limits
     Method 630 does not provide PCS isomer method detection limits or a
method for the determination of detection limits.  Due to the nature of
the analysis,  a rigorous method may not be possible.  However, in order
to better understand the meaning of the data and illustrate its
limitations,  estimated detection limits were derived.   They are stated in
the method to be in a working range of 1 ng to 10 ng.   Based on this
information,  and the information obtained from preliminary method
evaluation,  Versar's best estimates for detection limits of the PCS
homologs are  listed below.
             Estimated Detection Limits  for  the  PCS Homologs
                  Using Method  630  for Fly Ash Analysis
                      Isomer Group            ug/kg
                      Monochlorobiphenyls      0.2
                      Dichlorobiphenyls        0.3
                      Trichlorobiphenyls       0.4
                      Pentachlorobiphenyls     0.6
                      Hexachlorobiphenyls      0.6
                      Heptachlorobiphenyls     0.7
                      Octachlorobiphenyls      0.3
                      Nonachlorobiphenyls      0.9
                      Decachlorobiphenyl       1.0
                                   3-66

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     The  fly ash samples were extracted in two separate groups consisting
of samples from Facilities A and B, and from Facilities C and D,
respectively.  Extraction of the first group was begun on November 13,
and completed on November 17, 1986.  The remaining ash samples were
extracted November 18 through November 20.
     Sodium- sulfate was initially omitted from the extraction process.
No problems were observed during the method development from this
modification.  The extracts from the first group of samples (extracted
November  13) resulted in the formation of two layers upon concentrating.
In some instances, these layers could both be organic resulting in
partitioning of the analyte.  In addition, distinct layers in the extract
could be  a result of water.  Sodium sulfate was, therefore, incorporated
into all  further extractions.  An equal weight of sodium sulfate was added
to the soxhlet extractor; in addition, the extract was poured through a
sodium sulfate column into the Kudema-Danish (KD) flask.
     The  low surrogate recoveries of the carbon 13 monochlorobiphenyl and
tretrchlorobiphenyl for the extractions dated November 13 were a result
of the final concentration step.  The extract was transferred from the
ampule to a 1 ml conical vial.   The ampule was rinsed with 10 1 ml
aliquots.   Each rinse aliquot was blown down with nitrogen gas in a 1 ml
conical vial.  This probably resulted in the loss of lighter molecular
weight (higher vapor pressure)  congeners.   As a result,  a 5-ml conical
vial was used instead of the 1 ml vial.  In addition, an emphasis was
placed on passing a gentle stream of nitrogen over the extract.
Precipitation of crystals during the concentration step presented a
potential  problem with the absorption of the analyte to the crystalline
particulates.  To alleviate this problem,  the extract was passed through
a micro sodium sulfate column during the concentration.   The columns were
rinsed thoroughly with hexane to minimize  the loss of the analyte.
     Incorporating the modifications discussed, the technique used in all
extractions after November 13 was as follows.  The extract was
                                   3-67

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 concentrated to approximately 10 ml in a KD flask.  The extract and
 rinsings were passed through a pipette containing sodium sulfate into a
 50 ml centrifuge tube.  The extract was gently blown to 3 ml.  If the
 precipitation of particulates occurrad again, an additional filtering was
 performed.  The extract was then transferred to a 5 ml conical vial and
 gently concentrated to 50 ul.  During concentration, the sides of the
 vial were rinsed thoroughly.  Once concentrated to 50 ul, the vial was
 centrifuged to ensure the viscous extract collected exclusively at the
 bottom of the conical vial.
     Organic Constituents (BNA's) - The analysis for BNA's was performed
 on field water samples (i.e., quench water, ground water, and field
 leachates) and laboratory leachates contingent upon the results of the
 TOC and organic scan analyses.   If the TOG and/or organic scan results
 exceeded 5 rog/L for any of these samples, then, the sample was also
 analyzed for BNA's.
     Prior to initiating calibration or analysis, the standard mass
spectral abundance criteria were established for the GC/MS system.   This
was accomplished by analyzing a 50 ng injection of decafluorotriphenyl-
phosphene (DFTPP)  and tuning the system as necessary.  The criteria were
demonstrated daily or for each twelve-hour period of operation, whichever
was more frequent.   After the tuning criteria were established by using
DFTPP,  but prior to initiating sample analysis, the GC/MS system was
 initially calibrated using five standards that contained all the required
compounds.
     The organic constituents were determined by extracting the samples
with methylene chloride using a continuous extractor, and analyzing the
extract using gas  chronatography/mass spectrometry (GC/MS).  The
individual organic constituents were identified and quantified using
retention times and extracted ion current profiles.
                                   3-63

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 4.0  RESULTS AND DISCUSSION
      After the laboratory analyses  were  completed as detailed in
 Section 3.4,  the analytical results were summarized by sample matrix,
 analytical parameter,  and facility.  These  summaries include:  the
 facility operating  parameters  during sampling;  the analytical results  of
 each sample,  including blanks;  averages  and standard deviations of each
 analytical parameter by sample  matrix and facility;  and QC data,
 including relative  percent differences (RPDs) for each set of "blind"
 field duplicate  and laboratory  duplicate samples  and recoveries for
 spiked  samples.   These summary  tables were  evaluated to determine  any
 significant trends  in  the  data  between facilities,  sample  types (i.e.,
 matrices  ), shifts, and combustion  units.   The  summary tables and
 evaluations are  presented  in the following  sections.
      4.1   Facility  Operating Parameters
      During the  sampling activities  at each facility,  the  incinerator
 operator  recorded hourly operating  parameters.  These  operating
 parameters were  collected  to determine whether  differences  in the
 parameters significantly affect tha MWC  residue composition.   The
 operating data were used in an attempt to explain  significant differences
 between shifts of operation, combustion units,  and/or  facilities (see
 Section 5.3).  Tables  4.1, 4.2, 4.3, and 4.4 provide the operating
 parameters for Facilities A, B, C, and D, respectively.
     These tables include the unit,  date, shift, time, feed rate,  ram
 speed (related to feed rate), probe temperature, steam production  rate,
 combustion air, and electrostatic precipitator  (ESP) specifications.  The
 unit refers to the combustion unit number from which the samples were
 collected, while the date and shift refer to the date and shift of
operation during which the samples were collected.  The time  indicates
when the operating parameters were recorded.  The next parameter on the
table, feed rate, is expressed as both buckets and tons.  The buckets
 indicate the number of feed crane loads that were fed  into the charging
                                   4-1

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TABLE 4.1  SUMMARY OF FACILITY A OPERATING PARAMETERS
Feed Rate Ran Speed
Unit Date
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26


1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26
1 9/26


2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26


2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26
2 9/26


Shift
AM
AM
AM
AM
AM
AM
AM
AM


PM
PM
PM
PM
PM
PM
PM
PM


AM
AM
AM
AM
AM
AM
AM
AM


PM
PM
PM
PM
PM
PM
PM
PM


Tim (Buckets)
700
300
900
1000
1100
1200
1300
1400
TOTAL
AVERAGE
1500
1600
1700
1800
1900
2000
2100
2200
TOTAL
AVERAGE
700
300
900
1000
1100
1200
1300
1400
TOTAL
AVERAGE
1500
1600
1700
1800
1900
2000
2100
2200
TOTAL
AVERAGE
5
4
5
5
5
6
5
5
40
NA
6
5
5
4
4
3
4
0
31
NA
4
5
4
3
4
3
4
4
31
NA
4
4
5
3
5
4
6
0
31
NA
(tons)
3.5
2.8
3.5
3.5
3.5
4.2
3.5
3.5
28
NA
4.2
3.5
3.5
2.8
2.8
2.1
2.3
0
21.7
NA
2.3
3.5
2.8
2.1
2.3
2.1
2.3
2.8
21.7
NA
2.8
2.8
3.5
2.1
3.5
2.3
4.2
0
21.7
NA
(Units)
40
40
30
45
50
35
30
50
NA
40

20
0
0
30
30
20
40
NA
20
10
15
15
10
15
10
20
5
NA
12.5


20
10
15
30
10
20
NA
17.5
Probe
Temp.
Corijustlon Air
Steam Total Overflre
(F) (ib/hr) (Units) (Units)
1,000
980
1,100
1.000
1,320
1.060
1.380
1,020
NA
1.333

920
300
410
850
750
1,110
940
NA
826
1,100
1.C80
1.080
1,200
1,060
1,340
1.040
1.200
NA
1,100

1,120
1,300
1,000
1.020
1,350
1.080
1.110
NA
1,097
26,000
23,000
32.000
28,300
30.000
32.000
30,300
28.000
229.300
28,625

28,000
15,000
5.000
27,000
20.000
29,000
25.000
149,000
21,286
24,300
26,300
23,000
26.000
23.300
23.000
22,000
28.000
195.000
24.375

28,000
35,300
26,000
22.000
28,300
24.300
27,000
190,000
27.143
50
50
65
65
65
65
65
65
NA
61

70
0
0
70
70
70
70
NA
50
28
28
28
28
28
28
28
28
NA
28

30
28
30
30
32
32
30
NA
30
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA

NA
NA
NA
NA
NA
NA
NA
NA
NA
40
40
40
40
40
40
40
40
NA
40

0
0





HA
0
ESP (Outlet)
(Kv)
24
24
26
24
26
26
26
28
NA
26

22
23
22
22
25
26
23
NA
23
28
24
30

28
28
30
28
NA
28

25
28
28
29
24
28
30
NA
27
(«*)
160
160
200
120
120
240
240
320
NA
195

130
110
110
130
140
140
100
NA
123
400
300
440

450
260
460
240
NA
364

250
420
380
220
220
220
350
NA
294
4-2

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TABLE 4.2  SUMMARY OF FACILITY 3 OPERATING PARAMETERS
Feed Rat* Ram Speed
Unit Date Shift
3
3
3
3


3
3
3
3


4
4
4
4


4
4
4
4


9/28
9/28
9/28
9/28


9/29
9/29
9/29
9/29


9/28
9/28
9/28
9/28


9/29
9/29
9/29
9/29


AM
AM
AM
AM


PM
PM
PM
PM


AM
AM
AM
AM


PM
PM
PM
PM


Tim (Buckets) (tons)
300
1000
1200
1400
TOTAL
AVERAGE
1600
1800
2000
2200
TOTAL
AVERAGE
800
1000
1200
1400
TOTAL
AVERAGE
1600
1800
2000
2200
TOTAL
AVERAGE
19
19
19
19
76
NA
19
19
19
19
76
NA
21
21
21
21
34
NA
20
20
20
20
80
NA
13.3
13.3
13.3
13.3
S3. 2
NA
13.3
13.3
13.3
13.3
53.2
NA
14.7
14.7
14.7
14.7
58.8
NA
14
14
14
14
56
NA
(Units)
34
34
35
35
NA
34.5
25
28
34
33
NA
30
24
22

19
NA
21.7
19
22
23
27
NA
22.75
Probe
(F)
1,650
1,450
1,500
1,350
NA
1,488
1.425
1,300
1,250
1,400
NA
1,344
1,250
1,303
1,345
1,422
NA
1,330
1,373
1,369
1,241
1.251
NA
1,309
Stean
Corimstlon Air ESP
Total Overf 1re Zone #1 Zone »2
(Ib/hr) (Units) (Units)
30,000
30,000
80,000
30.000
320.000
30.000
30.000
80.000
76,000
84,000
320,000
80,000
99,000
100,000
99,000
100,000
398,000
99.500
105,000
109,000
105,000
94,000
413.000
103,250
45
30
45
45
NA
41
20
55
100
50
NA
56



42
NA
42
69
70
84
85
NA
77
27
27
24
23
NA
25
20
26
19
19
NA
21
22
22
22
22
NA
22
18
18
18
18
NA
18
(nA)
39
39
39
89
NA
39
89
89
89
89
NA
89
56
48
48
88
NA
60
24
28
24
16
NA
23
(oft)
107
107
107
107
NA
107
107
107
107
107
NA
107
104
104
104
92
NA
101
60
44
40
35
NA
45
                          4-3

-------
 hopper during the previous hour.  The tons were then calculated from the
 bucket number by using the approximate feed crane capacity.  The ram
 speed is also a relative measure of the feed rate, however, it is a
 relative measure of the feed rate into the incinerator, rather than into
 the charging hopper.  The charging ram (see Figure 3.1} forces the
 material from the charging hopper into the combustion chamber.  The probe
 temperature indicates the temperature in the incinerator, but because we
 are not aware of the exact probe location, it is a relative temperature
 and should not be directly compared between facilities.  The next
 parameter, steam production rate, indicates the pounds per hour of steam
 generated at the three energy recovery facilities.  The combustion air is
 a relative measure of the amount of air needed in excess of the
 stoichiometric requirement for complete combustion.  The combustion air
 can be either overfire, which is forced into the combustion chamber from
 above the combustion zone, or underfire, which is forced into the
 combustion chamber through the grates below the combustion zone.
 Finally,  the ESP specifications are relative measures of-the power
consumption by the ESP,  As the level of fly ash particulates in the flue
gas increase, the ESP power consumption must increase to maintain an
adequate removal efficiency.
     4.2  Solid Samples
     The solid samples collected included:  fly ash,  combined bottom/fly
ash, bottom ash, and landfill perimeter composite (i.e., disposed ash).
Each of these samples were analyzed for metals, PCBs, and PCDO/PCDFs, and
the results were summarized and evaluated.  Sections  4.2.1 through 4.2.3
present the analytical result tables for each parameter summarized by
sample matrix and facility and a narrative evaluation of these results.
     4.2.1  Metals
     The  solid samples were analyzed for total cadmium (Cd), chromium
 (Cr),  copper (Cu), iron (Fe), lead (Pb), manganese (Mn), nickel (Ni),
                                    4-6

-------
 zinc  (Zn), arsenic (As), selenium 
-------
                            TABLE 4.5  TOTAL METALS DATA FOR SOLID SAMPLES
                                             FLY ASH

Facility
A
A
A
A
A


B
a
a
a
a


c .
c
c
c
c


0
Sample
Description
Unit 1. 9/26. AM
Unit 1. 9/26. AM. Oup
Unit 1, 9/26, PM
Unit 2, 9/26. AM
Unit 2. 9/26. PM
FACILITY A AVERAGE
STANDARD DEVIATION
Unit 3, 9/28, AM
Unit 3. 9/28. AM, Oup
Unit 3, 9/29. PM
Unit 4, 9/28, AM
Unit 4, 9/29, PM
FACILITY B AVERAGE
STANDARD DEVIATION
Unit 2. 9/28. PM
Unit 2, 9/29. PM
Unit 2. 9/29. PM. Oup
Unit 2. 9/30. AM
Unit 2. 9/30, PM
FACILITY C AVERAGE
STANDARD DEVIATION
Unit 1-2. 10/3. AM
0 Unit 1-2, 10/3, AM, Oup
0
0
0


Unit 1-2, 10/3, PM
Unit 1-2, 10/4, AM
Unit 1-2, 10/4, PM
FACILITY 0 AVERAGE
STANDARD DEVIATION
Cd
mg/kg
193
186
215
222
138
190.3
29.6
322
316
251
381
475
349.0
75.3
107
191
157
223
188
173.2
39.1
259
172
286
210
206
226.6
40.6
Cr
ng/kg
79
66
57
66
76
70.8
5.6
105
98
74
97
100
94.3
10.3
76
54
52
48
49
55.3
10.3
77
67
93
89
90
83.2
9.8
Cu
mg/kg
2380
2040
1870
1250
1040
1716
499
745
724
588
912
854
765
112
1050
531
556
484
485
621
216
516
518
597
486
510
525
38
F«
ng/kg
17400
15000
9730
20200
15900
15646
3444
9900
9350
5960
16200
22300
12742
5812
9030
8200
8450
16700
14400
11356
3511
3320
7190
3790
8960
9170
8486
706
Pb
rag/kg
5550
5400
5660
5480
5090
5636
243
7350
7270
5280
9230
14400
3706
3109
3260
3490
3130
3420
2830
3226
234
5450
4600
5770
4740
4430
4998
519
Mn
mg/kg
1010
1020
1060
807
1090
997
99
895
389
824
1310
1070
998
176
320
388
382
341
353
357
25
857
751
1250
1410
1190
1092
248
N1
mg/kg
106
91
98
97
160
110
25
80
76
52
67
68
69
.10
130
102
95
245
212
157
61
63
55
36
89
36
76
14
Zn
mg/kg
15700
14500
15100
17400
9480
14436
2660
32700
31800
23600
34000
38800
32180
4923
10200
10300
8460
10600
9940
9900
750
22100
18600
23900
17600
17300
19900
2630
As
mg/kg
41.9
38.0
48.8
36.3
16.0
36.3
11.0
106
39.9
79.0
131
149
111.0
25.3
29.0
16.2
17.7
26.3
32.2
24.4
6.3
50.7
54.5
60.4
47.2
43.2
51.2
5.9
Se
mg/kg
<5
<5
<5
<5
<5
2.5
0
<10
<10
10.0
11.7
15.6
9.5
4.1
4.9
7.6
6.2
7.6
3.3
7.0
1.3
9.6
9.1
15.5
10.7
9.6
10.9
2.4
Hg
mg/kg
27
23
35
25
24
26.3
4.3
9.3
8.0
12
19
21
13.9
-5.2
1.3
5
4.0
3.1
1.4
3.0
1.5
1.3
2.0
1,4
0.94
l.Q
1.4
9.4
   TOTAL NUMBER           20      20
      MINIMUM            107      48
      MAXIMUM            475     105
  OVERALL AVERAGE        235    76.2
STANDARD DEVIATION        85    17.2
  20      20      20       20      20      20      20      20
 484    5960    2830      320      52    3460      16     2.5
2380   22300   14400     1410     245   38800     149    15.6
 907   12058    5642      861     103   19104    55.7     7.5
 550    4611    2534      335      49    8901    36.4     4.0
                                              4-8

-------
TABLE 4.5  TOTAL METALS DATA FOR  SOLID SAMPLES
                 COMBINED BOTTOM  AND FLY ASH

Facility
A
A
A
A
A


C
C
C
C
C


0
0
0
Sample •
Description
Unit I. 9/26. AM
Unit 1, 9/26, PM
Unit 2. 9/26, AM
Unit 2. 9/26. AM. Dup
Unit 2. 9/26, PM
FACILITY A AVERAGE
STANDARD DEVIATION
Unit 2, 9/28, PM
Unit 2, 9/29, PM
Unit 2. 9/30, AM
Unit 2. 9/30, AM, Oup
Unit 2. 9/30, PM
FACILITY C AVERAGE
STANDARD DEVIATION
Unit 1-2, 10/3. AM
Unit 1-2, 10/3, PM
Unit 1-2, 10/4, AM
0 Unit 1-2. 10/4. AM. Dup
0







Unit 1-2. 10/4, PM
FACILITY 0 AVERAGE
STANDARD DEVIATION
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION
Cd
ng/kg
17
13
17
IS
37
19.8
8.7
7.8
10
24
27
20
17.8
7.6
45
18
17
18
23
24.2
10.6
IS
7.8
45
20.6
9.5
Cr
ng/kg
25
19
12
16
12
16.8
4.9
22
332
19
26
37
87.2
122.6
38
28
31
36
43
35.2
5.3
15
12
332
46.4
76.9
Cu
ng/kg
452
387
369
377
193
356
86
329
5900
3420
608
5900
3231
2432
424
1060
289
728
524
505
269
15
193
5900
1397
1921
Fe
ng/kg
5130
6500
6650
9140
2100
5904
2300
5220
22300
5040
9720
16000
11656
6650
24500
3000
8590
95100
19000
31038
32638
15
2100
95100
16199
22073
Pb
mg/kg
633
585
2200
1140
1670
1246
619
259
6950
1700
1060
13200
4634
4884
3410
819
571
612
688
1220
1098
15
259
13200
2366
3324
Mn
ng/kg
281
331
134
251
188
247
56
110
339
155
1810
254
534
643
462
797
3130
640
544
1115
1014
15
110
3130
632
782
N1
ng/kg
21
30
22
24
13
22.0
5.5
44
556
42
38
93
154.6
201.7
37
25
26
119
82
57.8
37.0
15
13
556
78.1
131.0
In
ng/kg
1810
1480
1730
3050
1980
2010
544
545
1520
1570
3250
2980
1973
1005
2950
1920
2400
46000
2390
11132
17437
15
545
46000
5038
10971
As
ng/kg
6.1
2.9
7.9
12.2
4.7
6.8
3.2
4
4.7
5.7
7
22.8
3.8
.7-l
16.4
4.3
5.4
6.1
6.4
7.7
4.4
15
2.9
22.8
7.77
5.21
Se
ng/kg
<0.5
<2.S
<5
<5
<0.5
1.4
1.0
1.4
<5.
<5.
<0.5
<5.
1.8
0.9
<2.5
<1
<1
«l
<2.5
0.3
0.4
15
0.25
2.5
1.327
0.910
Hg
ng/kg
S.8
3.9
6.9
5.0
3.7
6.3
1.7
0.51
0.21
0.62
0.13
0.59
0.4
0.2
0.12
0.16
0.21
0.13
0.11
0.1
0.0
IS
0.11
8,7
2.276
2.980
                 4-9

-------
                                   TABLE 4.5  TOTAL METALS DATA FOR SOLID SAMPLES
                                                    BOTTOM ASH

Facility
8
3
3
B
3







Facility
Sample
Description
Unit 3, 9/28. AM
Unit 3. 9/29, PM
Unit 4. 9/28. AM
Unit 4, 9/28, AM, Oup
Unit 4. 9/29. PM
No.
M1n.
Max.
Avg.
Std. Oev.

Sample
Description
Cd
mg/kg
2.3
1.1
3.8
3.5
43
5
1.1
43
10.74
16.16

Cd
mg/kg
Cr
mg/kg
105
24
66
78
33
5
24
105
61.20
29.67

Cr
mg/kg
Cu
mg/kg
10700
7250
792
581
1720
5
581
10700
4209
4060

Cu
mg/kg
Fe
mg/kg
12000
27100
115000
24100
17500
5
12000
115000
39140
38290
LANDFILL
Fe
mg/kg
Pb
mg/kg
2920
1380
2140
3930
3630
5
1380
3930
2800
942
Mn
mg/kg
1520
430
1010
938
538
5
430
1520
887
387
N1
mg/kg
35
17
36
90
29
5
17
90
41.4
25.2
Zn
mg/kg
1930
914
2350
5760
12400
5
914
12400
4671
4194
As Se
mg/kg mg/kg
3.4 <5.
2.2 <5.
8.9 <5.
6.9 <5.
24.6 <5.
5 5
2.2 2.5
24.6 2.5
9.20 2.50
8.06 0.00
Hg
mg/kg
0.36
0.13
0.12
0.12
0.13
S
0.12
0.36
0.17
0.09
COMPOSITE
Pb
mg/kg
Mn
mg/kg
N1
mg/kg
Zn
mg/kg
As Se"
mg/kg mg/kg
Hg
mg/kf
C     Perimeter Composite       8.7




0     Perimeter Composite        30
85    1190   60600     709       572      120    4740     6.0      <5     0.5)




52     402   19600    1210       455      51    2050    14.3    <2.5     0.1$
                                                     4-10

-------
 although the metal concentrations were typically lower in the weathered
 ash  than in freshly generated ash, considerable metal concentrations
 remain  in the weathered ash suggesting that a major portion of the metals
 in the  ash may not be  readily mobile to the environment.
     Upon comparing the concentrations of metals in the fly ash to those
 in the  combined bottom/fly and bottom ash, some interesting observations
 arose.  First, the variability between shifts, units, and facilities was
 substantially higher for the combined and bottom ash than it was for the
 fly  ash.  In fact, the variability between shifts and units for the
 bottom/fly and bottom ash was greater than the variability between
 facilities for the fly ash.  This observation was expected because of the
 heterogeneous nature of the bottom/fly and bottom ash based on the
 diverse range of particle sizes compared to the more homogeneous nature
 of the  fly ash.   This heterogeneity made it extremely difficult to
 collect representative, comparable samples, as evidenced by the standard
 deviations.   Second,  the concentrations of cadmium, mercury, chromium,
 lead, nickel,  zinc, selenium, and arsenic were between 1.5 and ten times
 higher  in the fly ash than in the bottom/fly or bottom ash.   Third, the
 concentrations of copper and iron are approximately two times higher in
 the bottom/fly and bottom ash than they are in the fly ash.   Finally, the
 concentration of manganese is approximately equivalent for both ash
 fractions.
     4.2.2   Polychlorinated Biphenyls (PCBs)
     The solid samples were analyzed for individual PCB homologs and
 total PCBs.   The results of these analyses are tabulated and summarized
 in Table 4.6.
     A review of the  PCB homolog concentrations in the fly ash showed
 that the variability between shifts and units was relatively small, while
the variability  between facilities was relatively large.   Facility D had
the highest  concentration of total PCBs,  as well as the highest
concentration  of each individual PCB homolog,.followed by Facility B,
                                   4-11

-------
TABLE 4.6  PCBs IN SOLID SAMPLES
  FLY ASH


Plant
A
A
A
A
A


3
a
a
a
a


c
c
c
c
c
c
c
c


0
0
0
0
0









Sanple
Description
Unit 1, 9/26, AM
Unit 1. 9/26, AM, Oup
Unit 1. 9/26. PM
Unit 2, 9/26, AM
Unit 2. 9/26. PM
FACILITY A AVERAGE
STANDARD DEVIATION
Unit 3, 9/28, AM
Unit 3. 9/28, AM, Oup
Unit 3. 9/29, PM
Unit 4, 9/28, AM
Unit 4. 9/29, PM
FACILITY B AVERAGE
STANDARD DEVIATION
Unit 2. 9/28. PM
Unit 2. 9/29, PM
Unit 2, 9/29. PM. Oup
Unit 2. 9/30, AM
Unit 2. 9/30, PM
Unit 2, Coarst
Unit 2. Fine (ESP)
Unit 2, Hedlun
FACILITY C AVERAGE
STANDARD DEVIATION
Unit 1-2. 10/3, AM
Unit 1-2, 10/3, AM, Oup
Unit 1-2. 10/3. PM
Unit 1-2, 10/4, AM
Unit 1-2, 10/4, PM
FACILITY 0 AVERAGE
STANDARD DEVIATION
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION

MONO
-CB
ng/g



0.64

0.64
0.00


0.5

0.29
0.40
0.10












0.38
1.46
0.47
0.94
0.41
6
0.29
1.46
0.707
0.382

01
-CB
ng/g
0.7
0.73
1.37
0.13

0.73
0.44


2.01

0.38
1.19
0.32


0.31

0.49



0.65
0.16
2.88
2.42
5
7.37
1.34
4.00
2.21
13
0.13
7.87
2.048
2.111
4-12
TRI
-CB
ng/g


0.52


0.52
0.00


2.32
1.34
2.43
2.20
0.53










2.91
1.72
5.27
7.67
1.98
3.91
2.26
9
0.52
7.57
2.962
2.079

TETRA PENTA
-C8 -CB
ng/g ng/g









2.72 0.87
2.5
2.45
2.56. 0.37
0.12 0.00










2.41
1.02
2.16
5.52 2.25
1.31
2.48 2.25
1.60 0.00
8 2
1.02 0.87
5.52 2.25
2.511 1.560
1.270 0.690

TOTAL
PCS
ng/g
0.7
0.73
1.89
0.77
0
0.32
0.61
0
0
8.92
3.34
5.55
3.66
3.41
0
0
0.31
0
0.49
0
0
0
0.16
0.29
8.2
5.16
13.31
24.77
5.6
11.41
7.28
20
0
24.77
4.037
6.005


-------
        TABLE  4.6  PC3S IN SOLID SAMPLES
COMBINED BOTTOM AND FLY ASH


Plant
A
A
A
A
A

C
C
C
C
C

0
0
0
0
0






MONO
Saople -CB
Description ng/g
Unit 1. 9/20, AM
Unit 1. 9/26, PM
Unit 2. 9/26. AM
Unit 2, 9/26, AM, Oup
Unit 2. 9/26, PM
NUMBER OF PCBs FOUND 0
Unit 2, 9/28, PM
Unit 2. 9/29, PM
Unit 2. 9/30, AH
Unit 2, 9/30, AM, Oup
Unit 2, 9/30, PM
NUMBER OF PCBs FOUND 0
Unit 1-2. 10/3. AM
Unit 1-2. 10/3, PM
Unit 1-2, 10/4, AM
Unit 1-2, 10/4, AM, Oup
Unit 1-2. 10/4. PM
NUMBER OF PCBs FOUND 0
TOTAL NUMBER 0
MINIMUM NA
MAXIMUM NA
OVERALL AVERAGE NA
STANOARO DEVIATION NA
01
-CB
ng/fl

0.66



1





0



1.35
0.126
2
3
0.126
1.35
0.71
0.50
TRI
-CB
ng/g





0





0
0.35
5.66
2.79
14.3
9.52
5
5
0.35
14.3
6.52
4.94
TETRA PENTA TOTAL
-CB -CB PCS
ng/g ng/g ng/g
0
0.66
0
0
0
0 0 1
0
0
0
0
0
000
0.35
5.66
2.79
16.5. 32.15
9.646
1 0 3
1 0 15
16.5 NA 0
16.5 NA 32.15
16.50 NA 3.42
0.00 NA 8.13
          4-13

-------
                                     TABLE 4.6  PCBs IN SOLID SAMPLES
                                      BOTTOM ASH
                               MONO      01       TRI     TETRA    PEHTA    TOTAL
              Sample            -CB      -CB      -C8      -CB      -CB      PCS
Plant       Description        ng/g     ng/g     ng/g     ng/g     ng/g     ng/g

  B      Unit 3. 9/28. AN                                                        0
  8      Unit 3. 9/29, PH                       '                                 0
  3      Unit 4. 9/28, AN                                                        0
  3    Unit 4. 9/28, AN. Oup                                                     0
  3      Unit 4. 9/29. PM                                                        0

       NUMBER OF PCBs FOUND         030000
                                      LANDFILL COMPOSITE


                               MONO      01       TRI     TETRA    PENTA    TOTAL
              Sample            'CB      -C9      -CB      -CB      -CB      PCS
Plant       Description        ng/g     ng/g     ng/g     ng/g     ng/g     ng/g

  C     Perimeter Composite               41.5      225      109             375.5

  0     Perimeter Composite              0.689     2.36     1.54             4.589
                                        4-14

-------
 Facility A,  and Facility C, which had  the  lowest concentration of each
 PCS homolog.   The di-, tri-, and tetra-CB  horoologs were the moat
 prevalent and were of approximately equal  magnitude, while the mono- and
 Penta-CB homologs were also approximately  equal, but substantially  less
 prevalent than the di-, tri-, and tetra-CB homologs.  The higher
 chlorinated  PCS homologs (i.e., the PCB homologs more highly chlorinated
 than the Penta-CB class) were not detected in any fly ash sample.
     A review of the PCB data in Table 4.6 for the combined bottom/fly ash
 and bottom ash (Facility B) showed that only Facility 0 had measurable
 concentrations of PCBs in each sample.  Therefore, the variability  between
 facilities was significantly high.  Only one sample from Facility A
 (Unit 1,  9/26, PM) had a detectable, although minimal, PCB concentration
 of  0.66  ng/g.  Facilities B and C did not  have any samples in which PCBs
 were detected.  As was the case for the fly ash, the di-, tri-, and
 tetra-CB homologs were the most prevalent.  In fact, these were the only
 PCB homologs  detected in any of the combined ash samples.  The tri-CB
 homolog  was detected in all five samples from Facility D, while the
 tetra-CB homolog was detected in only one  sample from Facility 0.   The
 di-CB homolog was detected in two samples  from Facility 0 and in one
 sample from Facility A.
     The  landfill perimeter composite samples also contained only the
 di-, tri-, and tetra-CB homologs.   The PCB concentration of the landfill
 composite from Facility 0 was approximately equal to the PCB concentration
 in the combined ash samples from Facility D,  as expected.  However, the
 PCB concentration for the landfill composite from Facility C was the
 highest found in any sample (375.5 ng/g), yet the combined ash samples
 from this facility did not contain any detectable PCBs.   It was
anticipated that the results from Facility C would have exhibited the
 same trend noted for Facility D;  however, several different contributing
 factors may have caused this seemingly erroneous result from Facility C.
First,  an organic interference (see discussion of analytical procedures
 in Section 3.4.2)  in the  landfill  composite sample may have caused  an
                                   4-15

-------
 erroneously high PCS result for this sample.  Second, because of the
 heterogeneous nature of the disposed ash, some "pockets" of concentrated
 ash may have been sampled and subsequently biased the composite.  Third,
 an outside source of PCBs may have contaminated the ash once the residue
 had been placed in the disposal area.  One potential outside source of
 PCBs was the bulldozer or other diesel powered equipment used at the
 landfill.  Typically, this equipment uses hydraulic fluids that may
 contain PCBs.  If these hydraulic fluids were leaking, they may have
 contributed to the high concentration of PCBs in the landfill perimeter
 composite, especially since the bulldozer operates principally around the
 landfill's perimeter.
     Upon comparing the PCS concentrations of the fly ash with those of
 the combined and bottom ash, the following observations were noted.
 First, the variability between shifts, units, and facilities for the
 combined/bottom ash was substantially higher (i.e., where measurable
 quantities were detected) than for the fly ash.   This is due to the
 heterogeneity of the combined/bottom ash compared to the homogeneity of
 the fly ash.   Second, the PCS concentrations of the fly ash were
 significantly higher than those for the combined/bottom ash.  This
 indicates that the PCBs may condense on the fine fly ash particles or
 physically adhere to them and are negligible in the coarse bottom ash
material.   Third,  only the di-, tri-, and tetra-CB homologs were detected
 in both the fly ash and combined ash, and the mono- and penta-CB homologs
were found only in the fly ash.  This indicates that the bottom ash alone
 is not a source of mono- or penta-CB homologs,  and it dilutes the
concentration of these homologs below detectability in the combined ash.
This observation is supported by the bottom ash data for Facility B.
Finally,  Facility D had the highest concentrations of PCBs for both the
fly ash and combined ash, and Facility C had the lowest PCB concentrations
for both ash fractions.
                                   4-16

-------
      4.2.3   Polychlorinated Dibenzo-p-dioxins and Polychlorinated
             Dibenzo-furans (PCDD/PCDFs)
      The  solid  samples were analyzed  for  individual PCDD and PCDF
 homologs  in  the tetra- through octa-chlorinated classes.  Additionally,
 the  2,3,7,8-TCDD and 2,3,7,8-TCDF  isomers were identified and quantified.
 The  results  of  these analyses are  tabulated and summarized by sample
 matrix and facility in Table 4.7.
      A review  of the PCDD homolog concentrations in the fly ash showed
 that  the  variability of the homolog concentrations between units and
 shifts was relatively small, and the  variability of these concentrations
 between facilities was extremely large.  Facility C had the highest
 concentration of  total PCDOs, as well as the highest concentration of each
 PCDD  homolog.   Additionally, Facility C had the highest concentration of
 the 2,3,7,8-TCDD  isomer.  After Facility C, Facility B had the second
 highest concentration of each PCDD homolog, followed by Facility 0 and
 Facility A, which had the lowest concentration of each PCDD homolog.  The
 hexa-CDD homolog  was the most prevalent at three of the four facilities
 (it was the third most prevalent at Facility B), and the tetra-CDD
 homolog was the least prevalent at all four facilities.  Approximately
 5 percent of the  total tetra-CDDs was the 2,3,7,8-TCDD isomer.   Finally,
 one significant trend was noted, as the total PCDDs increased,  the hexa-
 through octa-chlorinated classes abundance increased disproportionately
 (i.e., when the total PCDD concentration was less than 500 ng/g, the
 hexa- through octa-chlorinated classes accounted for 70 percent of the
 total PCDD concentration, however,  when the total PCDD concentrations
 exceeded 500 ng/g, the hexa- through octa-chlorinated classes accounted
 for 90 percent of the total PCDD concentration).
     At Facility C,  two discrete fly ash fractions were also analyzed for
 PCDDs.  The first of these, the coarse fly ash (i.e.,  economizer ash),
 did not contain any detectable PCDDs.   However,  the second of these
fractions, the fine  fly ash (i.e.,  electrostatic precipitator ash),
contained the highest PCDD concentrations of any fly ash sample that was
                                   4-17

-------
TABLE 4.7  ?CDO AND PCOF IN SOLID SAMPLES
FLY ASH (OIOXIN  HOMOLOGS)


Plant
A
A
A
A
A


3
B
3
3
3


C
C
C
C
C
C
C


0
0
0
0
0








Sanple
Description
Unit 1. 9/26. AM
Unit 1, 9/26. AM. Oup
Unit 1. 9/26. PN
Unit 2. 9/26. AM
Unit 2. 9/26. PM
FACILITY A AVERAGE
STANDARD DEVIATION
Unit 3. 9/28, AM
Unit 3, 9/23. AM. Oup
Unit 3. 9/29. PM
Unit 4, 9/28. AM
Unit 4. 9/29. PM
FACILITY 8 AVERAGE
STANDARD DEVIATION
Unit 2. 9/28. PH
Unit 2, 9/29, PM
Unit 2. 9/29. PM. Oup
Unit 2. 9/30. AM
Unit 2, 9/30. PM
Unit 2, Coarse
Unit 2. Fine (ESP)
FACILTIY C AVERAGE
STANDARD DEVIATION
Unit 1-2, 10/3, AM
Unit 1-2. 10/3. AM, Oup
Unit 1-2. 10/3, PM
Unit 1-2. 10/4. AM
Unit 1-2, 10/4, PM
FACILITY 0 AVERAGE
STANDARD DEVIATION
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION
2.3.7,8
TOM
(ng/g)
0.093
0.11
0.13
0.24
0.22
0.16
0.06
0.38
0.38
0.63
0.24
0.13
0.35
0.17
2.2
l.S
2.1
2.4
1.5
<0.14
3.9
1.95
1.07
0.38
0.45
0.83
0.66
0.37
0.54
0.18
22
0.07
3.9
0.86
0.98
TETRA
-COO
(ng/g)
2.3
2.8
4.7
5.2
6.6
4.32
1.58
12
11
18
6.5
7.0
10.90
4.15
27
31
33
43
18
<0.14
38
27.2
13.3
5.2
5.1
19
11
7.9
9.64
5.15
22
0.07
43
14.3
12.2
PENTA
-COO
(ng/g)
11
14
20
16
32
18.60
7.31
139
114
137
84
99
114.60
21.34
238
710
722
513
335
<0.02
980
500
309
54
46
91
61
45
59.4
16.8
22
0.01
980
203
270
HEXA
-COO
(ng/g)
20
20
35
18
24
23.40
6.12
126
123
322
207
209
197
73
697
5565
3946
1430
1052
<0.03
3400
2299
1880
105
103
106
89
49
90.4
21.6
22
0.015
5565
802
1475
HEPTA
-COO
(ng/g)
14
14
26
14
14
16.40
4.80
100
93
203
352
435
237
136
331
1759
3030
1751
1089
<0.06
4900
1837
1559
45
48
81
39
37
50.0
16.0
22
0.03
4900
653
1199
OCTA
-COO
(ng/g)
17
18
31
13
11
18.00
6.99
96
39
210
586
1363
469
482
393
2460
3152
2338
1433
<0.16
2700
1782
1116
44
48
113
35
37
55.4
29.2
22
0.08
3152
690
1017
TOTAL
-COO
(ng/g)
64.J
68.8
116.7
66.2
87.6
80.7
19.8
473
430
890
1235.5
2113
1028
- 617
1686
10525
10883
6075
3927
0
12018
6445
4441
253.2
250.1
410
235
175.9
265
77.7
22
0
12018
2363
3775
             4-18

-------
                                      TABLE 4.7   PCOO  AND  PCOF  IN SOLID SAMPLES
                                      FLY ASH (FURAN HOMOLOGS)
Plant
  Sample
Description
  A      Unit 1. 9/26, AM
  A    Unit 1. 9/26, AM. Oup
  A      Unit I. 9/26. PM
  A      Unit 2, 9/26, AM
  A      Unit 2. 9/26. PM

        FACILITY A AVERAGE
        STANDARD DEVIATION

  B      Unit 3, 9/28, AM
  B    Unit 3. 9/28, AM. Oup
  3      Unit 3. 9/29, PM
  B      Unit 4, 9/28, AM
  B      Unit 4, 9/29. PM

        FACILITY B AVERAGE
        STANDARD DEVIATION

  C      Unit 2. 9/28. PM
  C      Unit 2, 9/29. PM
  C    Unit 2. 9/29. PM, Oup
  C      Unit 2, 9/30, AM
  C      Unit 2, 9/30. PM
  C       Unit 2, Coarse
  C     Unit 2.  Fine (ESP)

        FACILITY C AVERAGE
        STANDARD DEVIATION

  0     Unit 1-2. 10/3.  AM
  0   Unit 1-2,  10/3, AM, Oup
  0     Unit 1-2. 10/3,  PM
  0     Unit 1-2, 10/4,  AM
  0     Unit 1-2. 10/4.  PM

        FACILITY D AVERAGE
        STANDARD DEVIATION

           TOTAL NUMBER
              MINIMUM
              MAXIMUM
          OVERALL AVERAGE
        STANDARD DEVIATION
2,3.7,8
TCDF
(ng/g)



















0.66
26
13
13







2
0.66
26
13.33
12.6?
TETRA
-CDF
(ng/g)
20
23
34
52
39
43.6
25.3
91
97
107
48
59
80.4
22.3
61
164
169
130
73
3.3
110
102
55
36
36
93
70
53
57.6
21.7
22
3.3
169
73.6
43.2
PENTA
-CDF
(ng/g)
7.1
10
15
16
32
16.0
3.6
64
65
61
37
46
54.6
U.I
56
221
226
153
93
1.5
310
152
100
32
27
47
32
27
33.0
7.3
22
1.5
310
71.8
80.0
HEXA
-CDF
(ng/g)
17
14
23
96
13
33.6
31.3
56
61
241
41
54
90.6
75.5
54
336
2353
473
638
0.22
590
635
738
115
21
87
87
37
69.4
34.9
22
0.22
2353
246
496
HEPTA
-CDF
(ng/g)
14
12
22
44
9.9
20.4
12.5
40
40
19
49
63
42.2
14.3
10
32
77
666
610
<0.03
570
281
292
30
3.3
75
50
29
47.6
28.5
22
0.015
666
114
201
OCTA
-CDF
(ng/g)
2.1
2.3
4.0
1.4
2.0
2.4
0.9
8.1
3.3
21
11
34
16.5
9.9
24
60
362
108
175
<0.15
170
128
114
4.9
5.6
9.3
3.1
3.7
5.4
2.4
22
0.075
362
46
36
TOTAL
-CDF
(ng/g)
60.2
61.3
98
209.4
150.9
116.0
57.2
259.1
271.3
449
186
256
284
87.6
205
813
3187
1530
1589
5.52
1750
1297
1001
267.9
93.4
311.8
242.1
149.7
213
79.9
22
5.52
3187
552
765
TCOO r
TCDF
(ng/g)
124.5
13G.1
214.7
275.6
238.5
196.7
59.9
732.1
701.3
1339
1421.5
2369
1313
606
1891
11338
14070
7605
5516
5.52
13768
7742
5187
521.1
343.5
721.8
477.1
325.6
478
143
22
5.52
14070
Z915
4436
                                                  4-19

-------
                                      TABLE  4.7   PCOO  AND  PCOF  IN SOLID SAMPLES
                             COMBINED BOTTOM ASH  AND  FLY ASH  (DIOXIN HOMOLOGS)
Plant

  A
  A
  A
  A
  C
  C
  C
  C
  C
  Unit 1. 9/26.  AM
  Unit 1, 9/26.  PM
  Unit 2. 9/26.  AM
  Unit 2, 9/26.  PM

 FACILITY A AVERAGE
 STANOARO DEVIATION

  Unit 2. 9/28.  PM
  Unit 2. 9/29.  PM
  Unit 2. 9/30,  AM
Unit 2. 9/30. AM. Dup
  Unit 2. 9/30.  PM

 FACILITY C AVERAGE
 STANOARO DEVIATION

 Unit 1-2, 10/3. AM
 Unit 1-2, 10/3. PN
 Unit 1-2, 10/4, AM
 Unit 1-2. 10/4, PM

 FACILITY 0 AVERAGE
 STANOARO DEVIATION

    TOTAL NUMBER
       MINIMUM
       MAXIMUM
   OVERALL AVERAGE
 STANOARO DEVIATION
2.3,7,8
TCDO
(ng/g)
0.02
0.07
0.33
0.14
0.14
0.12
0.13
0.62
0.78
<0.31
0.36
0.28
0.07
<0.08
<0.23
0.04
0.07
0.04
12
0.02
0.78
0.21
0.24
TETRA
-COO
(ng/g)
1.5-
2.2
13
5.57
5.26
2.2
2
14
13
1.3
6.50
5.73
1.3
0.46
<0.23
1.1
0.75
0.47
12
0.14
14
4.35
5.23
PENTA
-OX)
(ng/g)
2.7
3.2
19
a. 30
7.57
11
11
47
50
10
25.8
13.6
4
2.3
1.9
2.6
2.70
0.79
12
1.9
50
13.7
16.3
HEXA
-COO
(ng/g)
1.9
2
11
4.97
4.27
13
18
67
78
11
37.4
29.0
3.4
1.4
1.5
1.8
2.03
0.31
12
1.4
78
17.5
25.3
HEPTA
-COO
(ng/g)
1.7
1.5
3.2
3.80
3.11
15
31
120
120
22
61.6
48.0
3.3
1.4
1.5
1.6
1.95
0.78
12
1.4
120
27.3
42.5
OCTA
-COO
(ng/g)
0.89
0.34
3.7
1.31
1.34
7.7
18
89
39
18
44.3
36.7
2.6
1.4
1.3
1-2
1.63
0.57
12
0.34
39
19.5
31.7
TOTAL
-COO
(ng/g)
8.69
9.74
54.9
24.44
21.54
48.9
80
337
350
62.3
176
137
14.6
6.96
6.2
3.3
9.02
3.31
12
6.2
350
82.3
119
                                                  4-20

-------
         TABLE 4.7   PCDO AND PCOF IN SOLID SAMPLES
COMBINED BOTTOM ASH  AM) FLY ASH (FURAN HOMOIOGS)

Plant
A
A
A
A


C
C
C
C
C


0
0
0
0







t
Saopl*
J.3,7,8
TCOF
Description (ng/g)
Unit 1. 9/26, AM
Unit 1. 9/26, PM
Unit 2, 9/26, AM
Unit 2. 9/26. PH
FACILITY A AVERAGE
STANDARD DEVIATION
Unit 2, 9/28, PN
Unit 2, 9/29, PM
Unit 2. 9/30, AM
Unit 2. 9/30, AM. Oup
Unit 2, 9/30, PM
FACILITY C AVERAGE
STANDARD DEVIATION
Unit 1-2. 10/3, AM
Unit 1-2. 10/3. PM
Unit 1-2, 10/4, AM
Unit 1-2. 10/4, PM
FACILITY 0 AVERAGE
STANDARD DEVIATION
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION
0.88

2.4
12
5.09
4.92
0.8
0.89
2.9
3.8
0.55
1.79
1.31
0.76
0.44
0.41
0.62
0.56
0.14
12
0.41
12
2.20
3.14
TETRA
-CDF
(ng/g)
6.3

20
91
39.10
37.12
5
4.7
20
24
3.4
11.42
8.75
5.1
3.1
2.3
3.4
3.48
1.02
12
2.3
91
15.69
23.90
PENTA
-CDF
(ng/g)
2.5

6.7
37
15.40
15.37
5.2
5.5
20
27
4.8
12.50
9.25
4.7
2
1.6
2.2
2.63
1.22
12
1.6
37
9.93
11.10
HEXA
-CDF
(ng/g)
1.3

3.2
18
7.50
7.47
6.4
11
24
•35
6.3
16.54
11.27
4.1
1.3
1.2
1.8
2.10
1.18
12
1.2
35
9.47
10.35
HEPTA
-CDF
OCTA
-CDF
(ng/g) (ng/g)
0.62

1.2
6.6
2.81
2.69
4.8
8
27
36
8.2
16.80
12.39
2.6
0.81
4.83
1.1
1.34
0.74
12
0.62
36
8.15
10.95
0.18

0.28
1.3
0.59
0.51
1.4
1.8
6.7
8.4
2.1
4.08
2.89
0.59
0.27
0.21
0.23
0.33
0.15
12
0.18
8.4
1.96
2.61
TOTAL
-CDF
(ng/g)
10.9

31.38
153.9
65.4
63.1
22.8
31
97.7
130.4
24.8
61.34
44.34
17.09
, 7.48
6.14
8.73
9.86
4.27
12
6.14
153.9
45.2
49.5
TCDD *
TCDF
(ng/g)
19.59

41.12
208.3
39.8
84.6
71.7
111
434.7
480.4
87.1
237
181
31.69
14.44
12.34
17.03
18.88
7.58
12
12.34
480.4
127
157
                   4-21

-------
TABLE 4.7  PCOO AND PCDF  IN SOLID SAMPLES
BOTTOM ASH (OIOXIN  HOMOLOGS)


Plant
3
8
B
B
3





Plant
B
B
B
a
B



Sanple
Description
Unit 3. 9/28. AM
Unit 3, 9/29, PM
Unit 4, 9/28. AN
Unit 4, 9/28. AM, Oup
Unit 4, 9/29. PM
FACILITY B AVERAGE
STANDARD DEVIATION


Samp]*
Description
Unit 3. 9/28, AM
Unit 3, 9/29. PM
Unit 4, 9/28. AM
Unit 4. 9/28. AM. Oup
Unit 4. 9/29, PM
FACILITY 8 AVERAGE
STANDARD DEVIATION
2.3.7.8
TCOO
(ng/g)
<0.04
<0.04
<0.08
0.01
<0.14
0.03
0.02

2.3.7,8
TCDF
(ng/g)
0.03
0.02
0.05
0.09
0.3
0.10
0.10
TETRA
-COO
(ng/g)
<0.04
<0.04
<0.08
0.11
0.65
0.17
0.24
BOTTOM ASH
TETRA
-CDF
(ng/g)
0.15
0.06
0.28
0.68
1.3
0.49
0.46
PENTA
-COO
(ng/g)
<0.01
<0.02
<0.05
0.21
2
0.45
0.78
(FURAN
PENTA
-CDF
(ng/g)
0.07
0.02
0.18
0.33
1.5
0.42
0.55
HEXA
-COO
(ng/g)
0.02
0.03
0.07
0.16
2.3
0.52
0.39
HOMOLOGS)
HEXA
-CDF
(ng/g)
0.02
0.05
0.1
0.26
2.5
0.59
0.96
HEPTA
-COO
(ng/g)
0.09
0.13
0.13
0.24
6.3
1.38
2.46

HEPTA
-CDF
(ng/g)
0.04
0.03
0.1
0.26
6.9
1.47
2.72
OCTA
-COO
(ng/g)
0.16
0.16
0.35
0.61
29
6.06
11.47

OCTA
-CDF
(ng/g)
<0.04
<0.04
0.06
0.12
3.7
0.78
1.46
TOTAL
-COO
(ng/g)
0.27
0.32
0.55
1.33
40.25
8.54
15.36

TOTAL
-CDF
(ng/g)
0.28
0.16
0.72
1.65
15.9
3.74
6.10











TCDO +
TCDF
(ng/g)
0.55
0.48
1.27
2.98
56.15
12.29
21.95
           4-22

-------
                                      TABLE 4.7  PCOO AND PCOF IN SOLID SAMPLES


                                      LANDFILL COMPOSITE (DIOXIH HOHOLOGS)


                              2.3.7.8   TETRA    PEHTA    HEXA     HEPTA    OaA     TOTAL.
              Sample           TCDO     -COO     -COO     -COO     -COO     -COO     -COO
Plant       Description       (ng/g)   (ng/g)   (ng/g)   (ng/g)   (ng/g)   (ng/g)   (ng/g)

  C     Perimeter Composite      0.07      1.2      5.7      6.3        9      6.1     28.8

  0     Perimeter Composite      0.15      2.5        6      4.1      4.2      3.9     20.7



                                      LANDFILL COMPOSITE (FURAN HOHOLOGS)
                              2.3.7.3   TETRA    PENTA    HEXA     HEPTA    OCTA     TOTAL   TCOO *
              Sample           TCOF     -CDF     -COF     -COF     -COF     -COF     -COF     TCOF
Plant       Description       (ng/g)   (ng/g)   (ng/g)   (ng/g)    (ng/g)   (ng/g)    (ng/g)   (ng/g)

  C     Perimeter Composite      0.51      2.4      3.9       4      3.3     0.81     14.41     43.21

  0     Perimeter Composite       1.3       11      7.7      5.3      2.7     0.61     27.31     48.01
                                                 4-23

-------
 analyzed.  This was expected because the chemical properties of the PCDD
 compounds cause then to adhere strongly to the finest particles.
     A  review of the PCDF homolog concentrations in the fly ash again
 showed  that the variability between the shifts and units was relatively
 small,  while the concentration variability between facilities was
 extremely large (i.e., the concentration standard deviations for the
 homologs exceeded the average homolog concentrations). Facility C had the
 highest concentration of total PCDFs, as well as the highest concentration
 of each PCDF homolog, followed by Facility B, Facility D, and Facility A,
 which had the lowest concentration of each ?CDF homolog.  The hexa-CDF
 homolog was the most prevalent at three facilities, and the second most
 prevalent at the fourth facility.  Similarly, the octa-CDF homolog was
 the least prevalent at three facilities and, the second least prevalent
 at the fourth facility.  The tetra-CDF homolog was generally the second
most prevalent, with the exception of Facility C where it was the least
prevalent.   As was the case for the PCDDs, the hexa- through octa-
chlorinated classes of PCDFs increased disproportionately as the total
PCDFs increased.
     As was the case for the PCDDs, two discrete fly ash fractions from
Facility C were analyzed for PCDFs.  Again, the coarse fly ash fraction
contained a minimal quantity of PCDFs,  but the fine fly ash fraction
exhibited the highest concentrations of PCDF homologs found in any fly
ash sample.   This was again anticipated because the PCDF compounds,
acting similarly to the PCDD compounds, adhere strongly to the finest fly
ash particles.
     Upon comparing the concentrations  of PCDDs with PCDFs in the fly
ash, the following observations were noted.  First, the total
concentrations of PCDDs and PCDFs followed the same sequence of abundance
among the facilities (i.e.,  the total concentrations of both PCDDs and
PCDFs increased in the order:   Facility A - Facility D - Facility B -
Facility C).   Second,  the production of the hexa-chlorinated classes of
PCDDs and PCDFs was favored at each of  the four facilities.  Third, the
                                   4-24

-------
 penta- and/or hepta-chlorinated classes of both PCDD  and  PCDF are never
 the most or least abundant.   Finally,  there does not  appear  to be any
 correlation between the relative abundances (i.e.,  percentage)  of PCDOs
 or PCDFs in the total  PCDD/PCDF concentrations.
      A review of the PCDD homolog concentrations in the combined
 bottom/fly ash and bottom ash showed that  the  variability between shifts
 and units was relatively small compared to the variability between
 facilities.   However,  some trends for  the  variabilities between shifts
 and units were observed.   At  Facility  A, variability  between units was
 very small (i.e.,  the  PCDD concentrations  of the ash  from the different
 units was essentially  equal),  but the  PM shift samples contained higher
 PCDD concentrations  than the  AM shift  samples.   Similarly, at Facility  B
 the PM shift  samples exhibited higher  PCDD concentrations than the AM
 shift samples,  but at  Facility B,  the  units  also showed a difference  with
 the samples from Unit  4  consistently having  higher  PCDD concentrations
 than those from Unit 3.   At Facility C. the  AM shift  samples  showed
 higher PCDD concentrations than the  PM shift samples.  Finally,  at
 Facility  D, the variability was  very small without  any notable  trends
 between shifts.
      As was the  case for  the  fly ash.  Facility C  combined ash samples had
 the  highest concentrations of  individual PCDD  homologs as well  as  total
 PCDDs. The samples from Facility A had the second highest PCDD  concentra-
 tions, followed  by the samples  from  Facilities D  and B, sequentially.
There was  not any notable trends for the relative abundances  of  the
 individual PCDD  homologs.  For  example, the penta-CDD homolog was  the most
abundant  for Facilities A and D, while  the octo-CDD and hepta-CDD  homologs
predominated at  Facilities B and C,  respectively.  Similarly,  the  least
abundant homolog was tetra-CDD for Facilities  B,  C, and D; however, the
octa-CDD homolog, which was the most abundant  at  Facility B,  was  the
least abundant at Facility A.   The 2,3,7,8-TCDD  isomer concentrations
were very low for all four facilities,   usually being only slightly above
the detection limit.
                                   4-25

-------
     A  review of the PCDP homolog concentrations in the combined
 bottom/fly ash and bottom ash samples indicated that the variability
 between shifts and units was relatively large, and that the variability
 between facilities was extremely large.  At Facility A, the samples from
 Unit 2  had higher PCDF concentrations than the samples from Unit 3, and
 the samples collected during the PM shifts had higher concentrations of
 PCDFs than those from the AM shifts.  Similarly, at Facility B the Unit 4
 samples exhibited higher PCDFs than the Unit 3 samples, and the PM shift
 samples contained more PCDFs than the AM shift samples.  However, at
 Facility C, the AM shift samples contained five times more PCDFs than the
 PM shift samples.  Finally, at Facility D the PCDF concentrations for the
 samples from each shift were essentially equal.
     The combined ash samples from Facilities A and C had the highest
 concentrations of PCDFs and were approximately equal and were seven times
 lower than corresponding concentrations from Facilities A and C.  The
 octa-CDF homolog was the least prevalent for three of the facilities;
 however, it was the second most abundant homolog for Facility B.  This
 difference may be attributed to the Facility B sample consisting .
 exclusively of bottom ash, while the samples from the other three
 facilities consisted of combined bottom/fly ash.  The tetra- and
hepta-CDF homologs predominated, each being the most abundant homolog at
 two facilities.   The concentrations of the penta- and hexa-CDF homologs
were approximately equal, and these homologs were never the most or least
abundant at any facility.  The 2,3,7,3-TCDF isomer accounted for 15 to
20 percent of the total tetra-CDF homologs.
     Upon comparing the PCDD and PCDF concentrations in the combined and
bottom ash,  the following observations were noted.   First, the
variabilities between shifts and units followed the same patterns for
PCDDs and PCDFs.   Second, there was not any correlation between the most
abundant or least abundant for PCDDs and PCDFs.  That is, while the
tetra-CDF homolog was the most abundant PCDF, the tetra-CDD homolog was
the least abundant PCDD.   One notable trend concerning the homologs was
                                   4-26

-------
 that the hexa-CDD and haxa-CDF homologs  were never the  most  or  least
 abundant.   Third, as  the total PCDDs  increased,  so did  the total  PCDFs.
 Consequently/  the facilities  that  had the  biggest  concentrations  of PCDDs
 had the highest concentrations of  PCDFs, and this  was also true for the
 facilities with the lowest  concentrations.   Finally, as was  the case for
 the fly ash,  there was not  an apparent correlation or trend  between the
 relative abundances of PCDDs  or PCDFs in the total PCDD/PCDF
 concentrations.
     A  review  of the  landfill composite sample results  for PCDDs  showed
 that Facilities  C and D were  approximately equal.   The  tetra-CDD  homolog
 was the least  abundant at both facilities,  and the hepta-CDD and
 penta-CDD  homologs were the most abundant  at Facilities C and D,
 respectively.  The tetra-CDOs at each facility were approximately six
 percent 2,3,7,8-TCDD.
     The PCDF  results  of the  landfill  composite  samples showed that
 Facility D was two times higher than  Facility C.   The oqta-CDF homolog
 was the  least "prevalent at each facility, and the  hexa-CDF and tetra-CDF
 homologs were  the most  prevalent at Facilities C and D,  respectively.
 There did not  appear  to be any trends  concerning the concentrations  of
 2,3,7,8-TCDF,  or  the  relative abundances of  PCDD or PCDF in  the total
 PCDD/PCDF concentrations.
     Upon comparing the PCDD  and PCDF  results of the combined bottom/fly
 ash with the landfill perimeter composite samples  from  Facilities C
 and D,   it was noted that the  combined ash from Facility C contained  six
 times more PCDDs and four times more PCDFs than  the landfill composite.
Conversely, at Facility D, the landfill composite  sample contained two
 times more PCDDs and five times more PCDFs than  the combined ash
 samples.  The first observation indicates that the landfill composite
 sample at Facility C may have been biased by bottom ash, or that  some of
the PCDDs and PCDFs may have already leached from  the landfill.    The
second observation suggests that the landfill composite sample at
Facility D may have been biased by fly ash, which  contained significantly
                                   4-27

-------
 more PCDDs  and  PCDPs than  the bottom or combined ash.  Similarly, both  of
 these discrepancies may be attributed to the heterogeneity of the
 combined  ash and disposed ash (i.e., landfill composite) samples.
      Upon comparing the PCDD and PCDF results of the fly ash with the
 combined  bottom/fly ash or bottom ash, the following observations were
 noted.  First,  the variability between facilities for both fly ash and
 combined/bottom ash PCDD and PCDF concentrations is extremely high.  This
 indicates that  the feed material and/or incinerator conditions at the four
 facilities are  very different, resulting in the formation of significant
 quantities of PCDD/PCDFs at one facility, and the formation of negligible
 quantities of PCDD/PCDFs at another.  Second, the variabilities between
 shifts and units for both PCDDs and PCDFs in the combined/bottom ash are
 greater than the corresponding variabilities for the fly ash.  This
 discrepancy is caused by the heterogeneicy of the combined/bottom ash
 compared to the homogeneity of the fly ash.  Third, the fly ash from
 three facilities contained from three to forty times more PCDDs than the
 combined ash,  and the fly ash from Facility B contained 120 times more
 PCDDs than the facility's bottom ash.   This indicates that the PCDDs are
associated with the fine fly ash particles and PCDD concentrations in the
bottom ash are minimal.   Therefore, the difference between the PCDD
concentrations in the fly ash and combined ash is caused by a bottom ash
dilution effect.  Similarly,  the fly ash from three facilities contained
 from two to 25 times more PCDFs  than the combined ash,  and the fly ash
from Facility  B contained 75  times more PCDFs than the  facility's bottom
ash.  Therefore, the difference  between PCDF concentrations in the
combined ash and fly ash is a result of the dilution effect from the
bottom ash.  Fourth,  the tetra-CDD homologs are the least prevalent in
both the fly ash and the combined/bottom ash, while the hexa- through
octo- chlorinated classes of  PCDDs are the most prevalent.  This suggests
that the typical incinerator  conditions favor the production of the more
highly chlorinated PCDD  species.   However,  for both the fly ash and
                                   4-23

-------
 combined/bottom ash, the tetra- through hexa-chlorinated species of PCDFs
 are the most abundant.  This indicates that these same incinerator
 conditions favor the formation of the lower chlorinated species of
 PCDFs.  Finally, the total concentrations of PCDDs and PCDFs in both fly
 ash and combined/bottom ash followed the same sequence of abundance among
 the facilities (i.e., the total concentrations of both PCDDs and PCDFs in
 fly ash and combined ash increased in the order:  Facility A - Facility D
 - Facility B - Facility C).
     4.3  Laboratory Leachates
     One laboratory leachate composite sample of fly ash and one of
 bottom/fly or bottom ash (plus 25 percent field duplicates) were
 collected from each facility.  These laboratory leachate composite
 samples were representative of all combustion units and shifts during
 which sampling was conducted.
     The laboratory leachate composite samples from each facility were
 subjected to three different leaching procedures in an attempt to
 evaluate and compare the mobility of various constituents under different
 extraction conditions..  The three different laboratory leaching
 procedures were Extraction Procedure (EP), Toxicity Characteristic
 Leaching Procedure (TCLP), and Mono-filled Waste Extraction Procedure
 (MWEP; SW-924).  The leachates prepared using these procedures were
 analyzed for metals and organic constituents.  Additionally, the leachates
 prepared using TCLP were analyzed for PCDD/PCDF.  The following sections
 present the analytical results for each parameter summarized by sample
 matrix, facility, and laboratory leaching procedure and a narrative
 evaluation of these results.
     4.3.1  Metals
     The laboratory leachates prepared by EP, TCLP, and MWEP were analyzed
 for cadmium (Cd), chromium (Cr), copper (Cu), iron (Fe), lead (Pb),
manganese  (Mn), nickel (Ni), zinc (Zn), arsenic 
-------
 by sample matrix, facility, and leachate procedure in Table 4.3.  The MWEP
 method  yielded  two leachates from each laboratory leachate composite sample.
 These leachates are listed in Table 4.8 as EX1 (i.e., Extraction 1) and EX2
 (i.e.,  Extraction 2).
     Upon reviewing Table 4.8, the following observations were noted.
 First,  the variability between leaching procedures and sample matrices
 appears to be much .greater than the variability between facilities.
 Additionally, because of this variability, there does not appear to be
 any trends between the metal concentrations and the facilities.  Second,
 zinc, iron, lead, and manganese were present in the highest concentrations
 in the leachates, while mercury was not present in any of the leachates.
 Third, the fly ash appeared to contain higher extractable quantities of
 cadmium and zinc than the bottom/fly and bottom ash, however the
 extractable quantities of chromium, iron, and lead in the bottom/fly and
 bottom ash were higher than in the fly ash.  Finally, the extractable
 quantities of copper,  manganese, nickel,  arsenic, mercury, and selenium
 were essentially equal in the fly ash and the bottom/fly or bottom ash.
     Upon comparing the different extraction procedures, the following
 observations were noted.   First, the EP and TCLP extraction methods were
 much more aggressive than the MWEP for leaching every metal, except
 selenium.   In fact,  the MWEP method was the only extraction procedure
 which leached selenium.  Second, none of  the extraction methods leached
mercury.  Third, the EP method appeared to extract copper and zinc more
 vigorously than the TCLP method, while the TCLP method extracted
chromium,  iron,  manganese,  nickel, and arsenic more aggressively than the
EP method.   In fact,  the TCLP method was  the only one to extract
arsenic.  Fourth,  the  extraction efficiencies of EP and TCLP were
approximately equal  for cadmium, lead, and zinc.   Finally, the
concentrations of metals in SW924-EX1 were generally greater than those
 in SW924-EX2.
                                   4-30-

-------
TABLE 4.3  EXTRACTABLE METALS DATA FOR THREE LABORATORY LEACHING PROCEDURES
Leachate
Procedure
EP Tox
Tap
SH924-EX1
SW924-EX2
EP Tox
TaP
SH924-EX1
SH924-EX2
EP Tox
TCLP
SM924-EX1
SW924-EX2
EP Tox
TttP
SW924-EX1
SW924-EX2
EP Tox
EP Tox
Tap
Tap
SM924-EX1
SH924-EX1
SW924-EX2
SW924-EX2
£P Tox
Tap
SW924-EX1
SW924-EX2
EP Tox
TCLP
SW924-EX1
SW924-EX2
EP Tox
EP Tox
TCLP
TCLP
SM924-EX1
SW924.EX1
SW924-EX2
SW924-CX2

Facility
A
A
A
A
c
c
c
c
0
0
0
0
B
B
3
a
A
A
A
A
A
A
A
A
3
3
3
3
C
C
C
c
0
0
0
0
0
0
0
0
Sample
Matrix
Bottom/Fly
Bottom/Fly
aottom/ny
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Sottom/Fly
Bottom/Fly
Sottom/Fly
Bottom/Fly
Bottom
Bottom
Bottom
Bottom
Fly
Fly (Oup.)
Fly
Fly (Oup.)
Fly
Hy (Oup.)
Fly
Fly (Dup.)
Fly
Fly
Fly
Fly
Fly
Fly
Fly
Fly
Fly
Hy (Dup.)
Fly
Fly (Oup.)
Fly
Fly (Oup.)
Fly
Fly (Oup.)
Cd
ng/L
0.327
0.682
<0.01
-0.01
0.060
3.32
«0.01
<0.01
0.649
0.025
<0.01
<0.01
0.368
0.418
<0.01
<0.01
6.02
7.72
0.015
0.032
«0.015
<0.01
<0.01
<0.01
18.0
17.2
<0.01
0.033
7.39
3.36
0.122
<0.01
3.60
9.18
10.3
3.90
0.015
<0.01
<0.01
<0.01
Cr Cu Fe
mg/L mg/L mg/L
0.016 1.19 4.50
0.096 0.019 60.6
<0.005 <0.005 <0.005
«0.005 «0.005 <0.005
0.0059 0.039 143
<0.005 0.0076 23.4

-------
TABLE 4.3  EXTRAaABLE METALS DATA FOR THREE LABORATORY LEACHING PROCEDURES
Leactiatt
Procedure
EP Tox



Tap



SH 924
Extract 1


SH 924
Extract 2


EP Tox



TCLP



SH 924
Extract I


SM 924
Extract 2


Sample
Type
Combined
Bottom/
Fly Ash

Combined
Bottom/
Fly Ash

Combined
Bottom/
Fly Ash

Combined
Bottom/
Fly Ash

Fly Ash



Fly Ash



Fly Ash



Fly Ash



Sumary
Statistics
Mln.
Max.
Avg.
Std Oev
Mln.
Max.
Avg.
Std Oev
M1n.
Max.
Avg.
Std Oev
M1n.
Max.
Avg.
Std Oev
Min.
Max.
Avg.
Std Oev
Mln.
Max.
Avg.
Std Oev
M1n.
Max.
Avg.
Std Oev
H1n.
Max.
Avg.
Std Oev
Cd
mg/L
0.06
0.827
0.481
0.289
0.025
3.32
1.111
1.296
0.005
0.005
0.005
0.000
0.005
0.005
0.005
0.000
6.02
18
9.568
3.395
0.015
17.2
7.468
6.006
0.005
0.122
0.027
0.043
0.005
0.033
0.010
0.010
.Cr
mg/L
0.0059
0.15
0.051
0.058
0.0025
0.439
0.135
0.130
0.0025
0.005
0.003
0.001
0.0025
0.0025
0.003
0.000
0.0025
0.038
0.008
0.013
0.0025
0.544
0.217
0.218
0.0025
0.114
0.035
0.042
0.0025
0.15
0.047
0.061
Cu
mg/L
0.039
1.19
0.352
0.485
0.0025
0.019
0.012
0.007
0.0025
0.07
0.026
0.026
0.0025
0.009
0.004
0.003
0.041
1.62
0.377
0.561
0.0025
0.201
0.070
0.072
0.0025
0.089
0.029
0.031
0.0025
0.012
0.005
0.004
Fe
mg/L
4.5
143
58.725
53.577
0.328
60.5
34.407
23.338
0.0025
0.038
0.311
0.015
0.0025
0.024
0.013
0.008
0.0025
0.49
0.096
0.177
0.0025
190
42.004
67.172
0.0025
0.167
0.041
0.061
0.0025
0.118
0.031
0.044
Pb
mg/L
2.09
34
16.038
12.419
0.655
30.1
13.539
11.032
0.025
C.063
0.035
0.016
0.025
0.025
0.025
0.000
4.72
25.2
16.237
6.654
0.025
15.2
3.216
6.029
0.025
0.128
0.044
0.038
0.025
0.148
0.053
0.046
Hn
mg/L
3.6
6.24
4.525
1.014
4.2
11.9
7.525
2.775
0.0005
0.0021
0.001
0.001
0.0005
0.0012
0.001
0.000
2.71
8.03
6.058
1.837
0.049
14.7
7.013
5.315
0.0005
0.014
0.005
0.004
0.0005
0.0052
0.002
0.002
Nl Zn
mg/L mg/L
0.241 38.5
0.415 726
0.311 221.150
0.071 291.610
0.346 23.3
0.305 373
0.549 133.325
0.168 139.706
0.0075 0.0015
0.0075 0.067
0.008 0.018
0.000 0.028
0.0075 0.0031
0.0075 0.051
0.008 0.019
0.000 0.020
0.137 186
1.92 726
0.570 404.000
0.611 171.624
0.0075 0.151
1.52 746
0.521 361.459
0.498 271.582
0 0.026
0.022 1.22
0.009 0.256
0.007 0.435
0.0075 0.0015
0.0075 1.2
0.008 0.221
0.000 0.439
As
mg/L
0.005
0.005
0.005
0.000
0.005
0.037
0.017
0.013
0.005
0.005
0.005
0.000
0.005
0.005
0.005
0.000
0.005
0.005
0.005
0.000
0.005
0.111
0.045
0.040
0.005
0.005
0.005
0.000
0.005
0.005
0.005
0.000
Hg Se
mg/L mg/L
0.004 0.025
0.004 0.025
0.004 0.025
0.000 0.000
0.004 0.0025
0.004 0.025
0.004 0.019
0.000 0.010
0.01 0.0025
0.01 0.025
0.010 0.011
0.000 0.009
0.01 0.0025
0.01 0.0025
0.010 0.003
0.000 0.000
0.004 0.025
0.004 0.025
0.004 0.025
0.000 0.000
0.004 0.0025
0.004 0.025
0.004 0.017
0.000 0.009
0.01 0.0025
0.02 0.108
0.012 0.039
0.004 0.034
0.01 0.0025
0.01 0.0125
0.010 0.009
0.000 0.005
                                    4-32

-------
TABLE 4.8  EXTRACTABLE METALS DATA FOR  THREE LABORATORY LEACHING PROCEDURES
            LEGEND:
                    EP  TOX  •  EP TOXICITY extraction procedure
                    TO?  -  TOTAL CHARACTERISTIC LEACHATE PROCEDURE
                    SW  924  -  Procedure for estimating monofllled solid waste leachate composition
                    SW  924  EX1 - First extract using SM 924 procedure
                    SW  924  EX2 • Second extract (on the sane sample) using SM 924 procedure
                    Bottom/Fly • combined bottom ash and fly ash samples
                    Fly - Fly ash
                    Bottom  •  Bottom ash
                    Oup.  -  Duplicate (split) of the previous sample
                                     4-33

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     4.3.2  Polychlorinated Dibenzo-p-dioxins and Polychlorinated
          •  Dibenzo-furans
     The laboratory leachata samples prepared by TCLP were analyzed for
 PCDD and PCDP homologs in the tetra- through octa-chlorinated classes.
 Additionally, the 2,3,7,8-TCDD and 2,3,7,8-TCDF isomers were identified
 and quantified.  The results of these analyses are summarized by facility
 in Table 4.9.
     A review of the PCDD and PCDF concentrations in the TCLP-prepared
 leachates showed that the extracted concentrations of PCDDs and PCDFs
 were approximately equal.  Only the hepta-CDD and octa-CDD homologs were
 detected in two fly ash leachates (Facilities A and B), and only the
 octa-CDD homolog was detected in one bottom ash leachate (Facility B).
 Similarly,  the hepta-CDF and octa-CDF homologs were detected in one fly
 ash leachate (Facility B), while only the hepta-CDF homolog was detected
 in the Facility A fly ash leachate.   The octa-CDF homolog was detected in
 only one bottom ash leachate (Facility B).  Because the solid samples
 contained significantly more PCDD and PCDF homologs than the
 TCLP-prepared leachates,  these observations indicate that the TCLP method
 is inefficient for extracting (i.e., leaching) PCDD and PCDF compounds in
 a waste ash matrix.   Furthermore, they indicate that only the highly
 chlorinated PCDD and PCDF species (i.e., hepta- and octa) tended to be
 extracted by TCLP.
     4.3.3   Organic  Constituents
     The laboratory  leachates prepared by EP,  TCLP,  and SW-924 (MWEP)
were analyzed for organic constituents (i.e.,  organic scan and BNAs).
Additionally,  the leachates  prepared by MWEP were analyzed for TOC.  The
 results of  these analyses are summarized by facility and extraction
procedure in Table 4.10.   The numerical code appearing with each organic
constituent  name represents  the CAS  designation for that compound.
                                   4-34

-------
                          TABLE  4.9   PCM AND PCOf  IN LABORATORY LEACHATE SAMPLES (TCLP)
                                               OIOXIN HONOLOGS
                                       2,3,7,8   TETRA    PEHTA    HEXA     HEPTA    OCTA   TOTAL
         Sanpl*          Sanple          TCOO     -COO     -COO     -CDO     -COO     -COO    -COO
Plant    Matrix        Description      (ng/1)   (ng/1)   (ng/1)   (ng/1)   (ng/1)   (ng/1)  (ng/1)
  A   Bottom/Fly   Unit 2. 9/26, AN
  A       Fly      Unit 2. 9/26, AN
        Bottom
          Fly
  C   Bottom/Fly
  C       Fly
      Bottom/Fly
          Fly
        Sample
Plant   Matrix
  A
  A

  B
  B

  C
  C

  0
  0
Bottom/Fly
    Fly

  Bottom
    Fly

Bottom/Fly
    Fly
             Unit 4, 9/28, AN
             Unit 4, 9/28, AN

             Unit 2, 9/29, PN
              Unit 2, Coarse

            Unit 1-2. 10/3, AN
            Unit 1-2. 10/3, AM
     Sanple
   Description

Unit 2, 9/26, AN
Unit 2. 9/26, AM

Unit 4, 9/28, AN
Unit 4, 9/28, AH

Unit 2, 9/29, PN
 Unit 2. Coarse
Bottom/Fly  Unit 1-2, 10/3, AM
    Fly     Unit 1-2, 10/3, AN
                     <0.038   <0.038   <0.023   <0.018   <0.028  <0.035       0
                     
-------
                      TABLE 4.10  EXTRACTABLE ORGANICS DATA FOR  THREE  LEACHING PROCEDURES
                                             EP Toxldty


lant
A
A
A
a
3
C
C
0
0
0

Sample
Matrix
Bottom/ Fly
Fly
Hy (Oup)
Bottom
Fly
Bottom/Fly
Fly
Bottom/Fly
Fly
Fly (Oup)
Organic
Scan
(mg/1)
<0.25
<0.25
<0.25
<0.25
<0.25
<0.25
<0.25
<0.25
<0.2S
<0.25
TOTAL NUMBER FOUND
                              BNA
                            Peaks
                            Found
                            (No.)

                                5
33
      Naphtti-     Methyl    Oletnyl-   Dimethyl   Methyoxy
        alene   Naphtha,   phthalate   pro'dlol     Ethane  Number of
        91203      91576       34662      126307   74498887    Unknown
       (ug/1)     (ug/1)      (ug/1)      (ug/1)     (ug/1)   Organic*
            8
18
16
                                                                13
                                                                IS

                                                                 9
                                                                18

                                                                16
                                                                17
                                                      12
                                           190
                                            23
                                                   TCL?
                              BNA   Dlethyl-   Olbutyl-   bis E.H.    Methyoxy    Methoxy   Dimethyl


lant
A
A
A
B
B
C
C
0
0
0

Sample
Matrix
Bottom/ Fly
Fly
Fly (Dup)
Bottom
Fly
Bottom/ Fly
Fly
Bottom/Fly
Fly
Fly (Dup)
Organic
Scan
(ng/i)
6.9
<0.25
<0.2S
<0.25
<0.2S
<0.25
<0.25
<0.25
<0.25
<0.25
                            Peaks    phthal.    phthal.
                            Found      84662      847*2
                            (No.)     (ug/1)     (ug/1)
TOTAL NUMBER FOUND
                               12
                               21
                               17
                               14

                               14
                               12
90
           21
           11
           16
           13

           10
           12
                            phthal.     Ethane
                             117817    74498887
                             (ug/1)     (ug/1)
                      22
                            Ethanol   Prop'dlol   Number of
                             111773      126307     Unknown
                             (ug/1)      (ug/1)    Organic*

                                                       11
                                            19
                                 13
                                 10
                                           140
                      10
                                            14
                                            11

                                            11
                                            10
                                                4-36

-------
                            TABLE 4.10  EXTRACTABLE  ORGANICS DATA FOR THREE LEACHING PROCEDURES
                                                   SW 924 FIRST EXTRACTION



Plant
A
A
A
8
3
C
C
0
0
0




Plant
A
A
A
8
8
C
C
0
0
0


Sample
Matrix
Bottom/Fly
Fly
Fly (Oup)
Bottom
Fly
Bottom/Fly
Fly
Bottom/Fly
Fly
Fly (Oup)
TOTAL NUMBER


Sample
Matrix
Bottom/Fly
Fly
Fly (Oup)
Bottom
Fly
Bottom/Fly
Fly
Bottom/Fly
Fly
Fly (Oup)


TOC
(•9/1)
9.4
4.3
6.3
12.1
16.9
10.3
9.2
31
6.7
4.4
FOUND
Oleyl
Alcohol
143282
(ug/1)
83









SNA
Organic Peaks
Scan Found
(rag/1) (No.)
<0.25 11
<0.2S
<0.25
<0.25 23
<0.2S
<0.2S 10
<0.2S
<0.25 6
<0.25
<0.25
SO
Etnoxy Cycloocta
Ethanol Decane
929373 17455139
(ug/1) (ug/1)
310 580


150






Benzole Dlethyl-
Phenol Add ph thai ate
108952 65850 84662
(ug/1) (ug/1) (ug/1)



28 46



3


1 1 1
Methoxy M.Furan- SW 924
Ethane dlone Extr. 1
74498887 766392 Unknowns
(ug/1) (ug/1) (No.)
4


10 6 17

10

3


                                                                                      £., 01M   Dimethyl
                                                                                      Oloxane   pro'diol
                                                                                     25796263     126307
                                                                                       (ug/1)     (ug/1)
                            Bis oxy
                            Ethanol
                             112276
                                                                                          510
                                                                                                                 96
                     160
TOTAL NUMBER FOUND
34
                                                     4-37

-------
                            TABLE 4.10  EXTRACTABLE ORGANICS  DATA  FOR THREE LEACHING PROCEDURES
                                                   SH 924 SECOND EXTRACTION



Plant
A
A
A
3
a
c
c
0
0
0


Sample
Matrix
Bottom/Fly
Fly
Fly (Oup)
Bottom
Fly
Bottom/Fly
Fly
Bottom/Fly
Fly
Fly (Oup)
SH 924
Extr. 2
TOC
(•9/1)
6.7
6.3
3.9
3.5
7.0
3.6
NA
NA
9.3
17.6
SH 924
Extr. 2
Org Scan
(ng/1)
<0.2S
<0.25
<0.25
<0.25
<0.2S
<0.25
<0.2S
<0.25
<0.2S
<0.25
SNA
Peaks
Found
(Ho.)
13


21

3
,
IS


Olethyl
Phenol phttial.
108952 34662
(ug/1) (ug/1)







33 3


                                                                           E.hexyl   Dimethyl
                                                                           phthal.   pro'dlol
                                                                             117817     126307
                                                                             (ug/1)     (ug/1)
                                                                                          Methoxy
                                                                                          Ethanol
                                                                                            111773
                                                                                            (ug/1)

                                                                                                6
                                                                                                      13
                                                                                          140
      TOTAL NUMBER FOUND
                                         57
Plant
  B
  B

  C
  C

  0
  0
  0
  Sample
  Matrix
  A    Bottom/Fly
  A       Fly
  A    Fly (Oup)
  Bottom
   Fly

Bottom/Fly
   Fly

Bottom/Fly
   Fly
Fly (Oup)
Bis oxy      Ethoxy    Beru.DI   Cycloocta
Ethanol     Ethanol  Carboxy.A      decane
  112276     929373     117828    17455139
(ug/1)       (ug/1)     (ug/1)      (ug/1)
                   18
      46
                Phenoxy   Oxahexa-
                Ethanol    decanol
                2315619   23778521   Unknowns
                 (ug/1)     (ug/1)      (No.)
                390
2       1200
         950
17
13
15
TOTAL NUMBER FOUND
                                                                        11
                                                                                     40
NOTE:
      Names of organic constituents abbreviated ;
      CAS numbers provided with constituent names
                                                      4-38

-------
     The  results for the EP-prepared leachates showed that the organic
 scan did  not detect any significant petroleum hydrocarbons in the samples
 from any  of the facilities.  The results also showed that similar BNAs
 were detected in samples from each facility with approximately equal
 concentrations.  Furthermore, every EP leachate that had a quantifiable
 BNA contained diethylphthalate, which was the predominant SNA.  Phthalate
 esters, such as the one described, are common plasticizers which were
 also noted in the laboratory leachate blank samples and therefore may
 represent a background interference.  The BNAs appeared to be slightly
 more abundant in the bottom/fly ash than in the fly ash.
     A review of the TCLP-prepared leachate results showed that gross
 measurement of petroleum hydrocarbon content was in one organic scan
 analysis  (bottom/fly ash. Facility A).  The other TCLP-prepared leachate
 results showed the same trends described above for the EP-prepared
 leachates.
     The results presented in Table 4.10 for the SW-924 leachates showed
 that there was not a predominant BNA compound.  The results also
 indicated that the bottom/fly ash and bottom ash contained slightly more
 leachable BNAs than the fly ash.  Finally, the results showed that there
 was essentially no difference between the first and second SW-924
 extractions.
     Upon comparing the results from the three different leaching
 procedures, the following observations were noted.  First, the TCLP
method appears to be more efficient for extracting BNAs than the EP
method (i.e.,  90 BNA constituents were detected in the TCLP leachates,
and only 33 BNAs were detected in the EP leachates).  However, for the
compounds that were extracted by both procedures (e.g., diethyl-
phthalate), the concentrations were approximately equal.  Second, the
extraction efficiency for SW-924 procedure appears to lie between the EP
and TCLP methods.   However, the SW-924 procedure extracted totally
different classes  of BNA constituents than the EP and TCLP methods.
Finally,  for  all three procedures, the combined bottom/fly ash and bottom
                                   4-39

-------
ash contained slightly more BNAs than their corresponding fly ash.
suggesting that the BNA compounds are associated with the coarser,
heavier bottom ash materials or may be completely destroyed as the fly
ash passes through high temperature zones in the incinerator.
     4.4  Field Water Samples
     The field water samples collected from each facility included:
ground water, quench water, and field leachate.  Each of these samples
were analyzed for total metals, PCBs. and BNAs.  Additionally, the quench
water and field leachate samples were analyzed for PCDD/PCDFs.  The
ground water samples were not analyzed for PCDD/PCDFs because these
materials generally absorb onto solid matrices which would not be
expected to migrate through the soil/ground-water interface.   Sections
4.4.1 through 4.4.4 present the analytical results of each parameter for
these samples summarized by sample matrix and facility, and a narrative
evaluation of the results.
     4.4.1  Metals
     The field leachates, ground water, and quench water samples were
analyzed for total cadmium (Cd), chromium (Cr), copper (Cu),  iron (Fe),
lead (Pb), manganese (Mn), nickel (Ni), zinc (Zn), arsenic (As), selenium
(Se), and mercury (Hg).   The results of these analyses were summarized by
sample matrix and facility and are presented in Table 4.11.
     A review of the field leachate data in Table 4.11 showed that the
variability between samples at each facility, as well as the  variability
between facilities, is relatively high.  However, the variability between
samples at Facility D was lower than that at the other two facilities.
In general. Facility C leachates contained the highest concentrations of
metals, while the leachates at Facility B contained the lowest
concentrations of metals.  Iron was the most prevalent metal  tested,
while mercury and selenium were the least concentrated metals.
     A review of the ground water data indicated that the variabilities
between samples and facilities were relatively small.  Furthermore, the
                                   4-40

-------
                                  TABLE 4.11  TOTAL METALS DATA FOR  FIELD  WATER SAMPLES
                                                      FIELD LEACHATES
Facility

   B
   8
   3
Sample
Description
Cast Sid*
North Sid*
Northeast Corner
FACILITY 3 AVERAGE
STANOARO DEVIATION
North Side
Northeast Corner
Northwest Corner
FACILITY C AVERAGE
STANOARO DEVIATION
Northeast Corner
Northeast Corner, Oup
Southeast Corner
FACILITY 0 AVERAGE
STANADARD DEVIATION
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANOARO DEVIATION
Cd
(mg/D
<0.010
<0.010
0.044
0.0180
0.0184
<0.010
<0.050
<0.010
0.0117
0.0094
0.031
0.023
<0.005
0.0188
0.0120
9
0.0025
0.044
0.0162
0.0142
Cr
(ng/D
<0.005
<0.005
0.024
0.0097
0.0101
0.011
0.914
0.0053
0.3101
0.4270
0.13
0.099
0.069
0.0993
0.0249
9
0.0025
0.914
0.1397
0.2773
Cu
(mg/L)
0.112
0.089
0.091
0.0973
0.0104
0.2
2.57
0.045
0.9383
1.1555
0.762
0.603
0.222
0.5290
0.2266
9
0.045
2.57
0.522
0.762
Fe
(
-------
                                   TABLE 4.11   TOTAL METALS DATA FOR FIELD WATER SAMPLES
                                                      QUENCH WATER
                Sample
Facility      Description

   A         Unit 1.  9/26
   A         Unit 2.  9/26

          FACILITY A  AVERAGE
          STANDARD DEVIATION
   8         Unit 3,  9/28
   3         Unit 4.  9/28
   3       Unit  4,  9/28,  Oup

          FACILITY 8  AVERAGE
          STANDARD DEVIATION
   C         Unit 2.  9/28
   C         Unit 2.  9/30

          FACILITY C  AVERAGE
          STANDARD DEVIATION
   0         Unit 2,  10/3
   0       Unit  2.  10/3, Oup
   0         Unit 2.  10/4

          FACILITY 0  AVERAGE
          STANDARD DEVIATION
             TOTAL  NUMBER
                MINIMUM
                MAXIMUM
            OVERALL AVERAGE
          STANDARD  DEVIATION
Cd
(mg/L)
0.065
0.114
0.0895
0.0245
<0.005
<0.005
<0.005
0.0025
0.0000
0.214
0.042
0.1280
0.0860
0.795
1.3
1.91
1.3350
0.4559
10
0.0025
1.91
0.4448
0.6369
Cr
(mg/L)
0.018
0.013
0.0155
0.0025
0.04
0.0085
0.0085
0.0190
0.0148
0.0098
0.014
0.0119
0.0021
0.408
0.646
1.12
0.7247
0.2959
10
0.0085
1.12
0.2286
0.3631
Cu
(mg/L)
0.117
0.253
0.185
0.068
0.02
0.048
0.041
0.0363
0.0119
0.066
0.064
0.0650
0.0010
2.51
3.36
13.1
6.4900
4.7064
10
0.02
13.1
2.008
3.906
Ft
(mg/L)
1.21
1.75
1.48
0.27
0.037
0.409
0.348
0.2647
0.1629
3.301
2
1.4005
0.5995
35
56.2
141
77.4000
45.7972
10
0.037
141
23.88
43.10
Pb
(mg/L)
4.07
5.94
S.005
0.935
0.176
0.274
0.264
0.2380
0.0440
0.213
0.289
0.2510
0.0380
19.1
27.8
37.9
28.2S67
7.6822
10
0.176
37.9
9.503
13.054
Mn
(mg/L)
0.144
0.127
0.1355
0.0085
0.024
0.082
0.079
0.0617
0.0267
' 0.6
0.34
0.7200
0.1200
7.47
12.6
10.6
10.2233
2.1112
10
0.024
12.6
3.257
4.712
N1
(mg/L)
<0.018
<0.018
0.009
0
<0.018
<0.018
<0.018
0.0090
0.0000
0.078
0.139
0.1085
0.0305
0.19
0.322
0.349
0.4537
0.2847
10
0.009
0.349
0.1623
0.2496
Zn
(mg/D
4.69
6.26
5.475
0.785
0.087
0.218
0.203
0.1693
0.0585
9.67
7.04
8.3550
1.315Q
64.6
132
192
129.53
52.04
10
0.087
192
41.68
64.26
AS

Se
(mg/L) (mg/L)
<0.010
0.017
0.011
0.006
<0.010
<0.010
<0.010
0.0050
0.0000
<0.010
<0.010
0.0050
0.0000
0.202
0.267
0.542
0.3370
0.1474
10
0.005
0.542
0.1058
0.1716
<0
<0


<0
<0
<0
0
0
<0
<0
0
0
<0
<0
<0
0
0

0
0
0
0
.0125
.0125
0.005
0
.0125
.0125
.0125
.0050
.0000
.0125
.0125
.0050
.0000
.0125
.0125
.0125
.0050
.0000
10
.0125
.0125
.0125
.0000
Hg
(rag/L)
0.0054
0.013
0.0117
0.0063
<0.0002
0.001
0.00099
0.0007
0.0004
0.00032
0.00032
0.0003
0.0000
0.022
0.02
0.0039
0.0153
0.0081
10
0.0001
0.022
0.0072
0.0086
                                                       4-42

-------
                                TABLE 4.11  TOTAL METALS DATA FOR FIELD HATER SAMPLES
                                                    GROUNOHATER
Facility      Description

   A              *1
                               Cd      Cr      Cu      F«      Pb      Hn       HI       Zn      As      S«      Hg
                             (mg/L)  (mg/L)  (mg/L)  (rag/L)   (mg/L)   (mg/L)    (mg/L)   (mg/L)   (mg/L)   (mg/L)  (mg/L)

                             
-------
concentrations of metals in the ground water were almost negligible, with
only manganese and iron ever exceeding the 1 mg/L level.  Mercury/ lead,
selenium, and nickel were not found in any ground water samples, and
cadmium and arsenic were found in only one sample, each.  Iron was the
predominant metal detected, followed sequentially by manganese, zinc,
copper, chromium, arsenic, and cadmium.
     A review of the quench water data showed that the variabilities
between shifts and/or units were very small, except for Facility 0 where
they were substantially higher.  This observation was expected since the
quench water samples from Facility 0 contained much higher quantities of
solids than the samples from the other facilities.  The variability
between facilities was relatively large.  Facility D had the highest
concentration of every metal in the quench water, while Facility 3
had the lowest concentrations for nine out of the eleven metals.  Iron
and zinc were the most concentrated metals in the quench water, followed
closely by lead, while mercury was the least concentrated metal.
     Upon comparing the analytical results of the field leachates, ground
water, and quench water, the following observations were noted.  First, the
quench water contained the highest concentration of metals, followed by
the field leachate and ground water, sequentially.  Second, there did not
appear to be any correlation between the field leachate and ground water
data for any given facility.  Third, the quench water and field leachate
results from Facility B are comparable, while the quench water metals
concentrations from Facility 0 are an order of magnitude higher than the
field leachate results.  No similar trends for Facility C were observed.
Finally, although Facility B had the lowest metals concentrations in its
quench water and field leachate, it had the highest concentrations in its
ground water (no background metals data was available for comparison).
     4.4.2  Polychlorinated Biphenyls
     The field leachates, quench water, and ground water samples were
analyzed for individual PCB homologs and total PCBs.  The results of
                                   4-44

-------
 these  analyses are summarized by sample matrix and facility and are
 presented  in Table 4.12.  A  review of this table shows that only
 negligible concentrations of PCBs were detected, with the highest total
 PCS  concentration for any sample being only 0.03 ug/L.  Additionally,
 only the three lowest chlorinated classes of PCBs (i.e., mono-, di-, and
 tri-)  were detected.
     4.4.3 Polychlorinated Dibenzo-p-dioxins and Polychlorinated
            Dibanzo-furans
     The field leachate and quench water samples were analyzed for PCDDs
 and  PCDFs  in the tetra- through octa-chlorinated classes.  Additionally,
 the  2,3,7,8-TCDD and 2,3,7,3-TCDF isomers were identified and
 quantified.  The results of these analyses are summarized by sample
 matrix and facility in Table 4.13.
     A review of the PCOO homolog concentrations in the field leachates
 showed that the variabilities between samples at a given facility and
 between facilities were both extremely high (i.e., the standard
 deviations of the results exceeded the averages).  Because the field
 leachate samples at a given facility were collected within 100 to
 200 feet of each other, this variability between samples at a given
 facility was not anticipated.  Two possible explanations for these
 observed differences are (1) some of the samples appeared to be natural
 seeps  (i.e., "true" field leachate) that were turbid and expected to
 contain more leachable constituents than the other samples, which
 appeared to be surface water runoff, and (2) the heterogeneity of the
 disposed ash materials may have caused "pockets" or areas of more highly
 contaminated ash located in random areas of the landfill.  The leachates
 from Facility C contained the highest concentrations of PCDDs, and the
 leachates from Facilities B and 0 had approximately equal PCOD
 concentrations which were less than those from Facility C.  The hepta-CDD
homolog was the most abundant, and the tetra-CDD homolog was the least
abundant.   The 2,3,7,8-TCDD isomer accounted for 6 percent of the
tetra-CDD homologs and 0.4 percent of the total PCDDs.
                                   4-45

-------
                                  TABLE 4.12  PCBs IN FIELD WATER  SAMPLES
                                      FIELD LEACHATE
Plant

  B
  B
  B

Sample
Description
MONO
-C8
ug/L
DI
-CB
ug/L
TRI
-•:B
ug/L
TETRA
-CB
ug/L
PENTA
-CB
ug/L
TOTAL
PCB
ug/L
             East Side
            North Sldt
         Northeast Corner
  C         North Side
  C      Northeast Corner
  C      Northwest Corner

  0      Northeast Corner
  0    Northeast Corner,  Oup
  0      Southeast Corner

       NUMBER OF PCBs FOUND
                                         0.302
                                                  0.008

                                                      1
    0
    0
    0

0.002
    0
    0

    0
    0
0.008
                                      GROUNOWATER
Plant

  C
  C
  C
  C
              Sample
            Description
                #4
          Production Well

       NUMBER OF PCBs FOUND
MONO
-CB
ug/L




01
-CB
ug/L




TRI
-CB
ug/L




TETRA
-CB
ug/L




PENTA
-CB
ug/L




TOTAL
PCB
ug/L
0
0
0
0
                                       4-46

-------
                           TABLE 4.12  PCBs IN FIELD WATER SAMPLES
                              QUENCH HATER


Plant
A
A
B
3
B
C
c
0
0
0

Sampl*
Description
Unit i, 9/26
Unit 2. 9/26
Unit 3. 9/28
Unit 4, 9/28
Unit 4, 9/28. Oup
Unit 2. 9/28
Unit 2. 9/30
Unit 2. 10/3
Unit 2. 10/3, Oup
Unit 2, 10/4
MONO 01 TRI TETRA PENTA TOTAL
-C8 -CB -CB -CB -C8 PCS
ug/L ug/L ug/L ug/L ug/L ug/L
0
0.004 ' 0.004
0
0
0.03 0.03
0
0.02 0.02
0
0
0
NUMBER OF PCBs FOUND
                                 4-47

-------
                                   TABLE 4.13  PCDO AND PCDF  IN FIELD WATER SAMPLES
                                      FIELD LEACHATE (DIOXIN HOMOLOGS)

Sanple
Plant Description
B
B
8
C
C
C
0
0
0
East Side
North Side
Northeast Corner
North Side
Northeast Corner
Northwest Corner
Northeast Corner
Northeast Corner, Oup
Southeast Corner
2.3.7.8
TCDO
(ng/D
<0.06
<0.48
0.28
<0.22
1.6
<0.05
<0.22
<0.26

TETRA
-COO
(ng/1)
<0.06
<0.48
6.6
<0.22
28

-------
TABLE 4.13  POM AND PCOF  IN  FIELD MATER  SAMPLES
    QUENCH MATER (DIOXIN HOHOLOGS)


Plant
A
A
B
3
C
C
0
0
0






Sanple
Description
Unit 1, 9/26
Unit 2. 9/26
Unit 4. 9/28
Unit 4. 9/28. Oup
Unit 2. 9/28
Unit 2. 9/30
Unit 2. 10/3
Unit 2, 10/3, Oup
Unit 2. 10/4
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION
2.3.7.8
TCDO
(ng/1)
<0.08
<0.08
<0.07
<0.07
<0.17
<0.81
8.2
17
1
9
0.035
17
2.98
5.55
TETRA
-COO
(ng/1)
0.1
2
<0.07
<0.07
<0.17
0.59
190
700
24
9
0.035
700
102
219
PENTA
-COO
(ng/D
0.82
4
«0.03
<0.05
0.26
5.9
610
650
30
9
0.015
650
150
258
HEXA
-COO
(ng/1)
0.66
2
<0.01
<0.04
1.1
10
500
450
72
9
0.005
500
115
194
HEPTA
-COO
(ng/D
0.58
1.9
<0.03
0.05
1.5
19
450
420
77
9
0.015
450
108
177
OCTA
-COO
(ng/1)
0.43
0.98
0.06
0.13
1.2
12
250
330
53
9
0.06
330
72
119
TOTAL
-COO
(ng/D
2.59
10.88
0.06
0.18
4.06
47.49
2000
2550
306
9
0.06
2550
547
937
    QUENCH MATER (FURAN HOHOLOGS)


Plant
A
A
8
B
C
C
0
0
0







Sample
Description
Unit 1. 9/26
Unit 2. 9/26
Unit 4; 9/28
Unit 4. 9/28. Oup
Unit 2. 9/28
Unit 2. 9/30
Unit 2. 10/3
Unit 2. 10/3, Dup
Unit 2. 10/4
TOTAL NUMBER
MINIMUM
MAXIMUM
OVERALL AVERAGE
STANDARD DEVIATION

2.3,7,8
TCOF
(ng/1)
0.27
2.1
<0.06
<0.08
0.14
0.55
110
99
14
9
0.03
110
25.1
42.7

TETRA
-CDF
(ng/D
1.7
12
<0.06
<0.08
0.98
2.4
640
590
91
9
0.03
640
149
251

PENT*
-COF
(ng/1)
0.91
6.1
«0.01
<0.04
0.76
4
560
460
33
9
0.005
560
124
209
4-49
HEXA
.COF
(ng/D
0.51
3.1
<0.01
<0.02
0.61
6.2
490
390
31
9
0.005
490
108
131

HEPTA
-CDF
(ng/D
0.36
1.2
<0.02
0.04
0.52
6.5
310
280
59
9
0.01
310
73
120

OCTA
-CDF
(ng/D
0.27
0.27
<0.15
<0.30
0.25
1.4
75
68
16
9
0.075
75
18
29

TOTAL
-CDF
(ng/D
4.02
24.77
0
0.04
3.12
20.5
2075
1788
330
9
0
2075
472
790

TCDO *•
TCDF
(ng/D
6.61
35.65
0.06
0.22
7.18
67.99
4075
4338
636
9
0.06
4338
1019
1716


-------
     The PCDF homolog concentrations in the field leachates again showed
that the variabilities between samples at a given facility and between
facilities were both extremely high.  The leachates from Facility C
contained the highest PCDF concentrations, followed by the leachates from
Facilities B and 0, sequentially.  The concentrations of the tetra-,
penta-, and hexa-CDF homologs were approximately equal, and these three
homologs were the most abundant.  The octa-CDF homolog was the least
abundant.  The 2,3,7,3-TCDF isomer accounted for 15 percent of the total
tetra-CDFs and 5 percent of the total PCDFs.
     Upon comparing the results of the PCDDs with the PCDFs in the field
leachate samples, the following observations were noted.  First, the
leachates from Facility C contained the highest concentrations of both
PCDDs and PCDFs, and the leachates from Facilities B and 0 contained
approximately equal concentrations of both PCDDs and PCDFs.  Second, the
abundances of the tetra-CDD and tetra-CDF homologs appeared to be
inversely proportional (i.e., the least abundant PCDD homolog and the
most abundant PCDF homolog).  Third, the abundances of the octa-CDD and
octa-CDF homologs also showed this inverse proportionality.  Finally,
there did not appear to be any correlation between the relative
abundances of PCDDs or PCDFs in the total PCDD/PCDF concentrations.
     The PCDD results for the quench water showed that the variability
between shifts and units was relatively small compared to the variability
between facilities.  This suggests that the different combustion
conditions and feed materials at each facility contribute to this
variability.  The quench water samples from Facility D contained the
highest PCDD concentrations, followed by the quench water samples from
Facilities C and B, sequentially.  There did not appear to be any
correlations for the least or most abundant homologs, or for the
2,3,7,3-TCDD isomer.
     A review of the PCDF concentrations in the quench water again showed
that the variability between shifts and units was relatively small
compared to the variability between facilities.  The quench water from
                                   4-50

-------
 Facility D contained the highest PCDP concentrations,  followed by the
 quench water samples from Facilities C and B,  sequentially.   Again,  there
 did not appear to be any trends for the least  or most  abundant homologs,
 or for the 2,3,7,8-TCDF isomer.
      For quench water,  comparing the PCDD results with the PCDF results
 indicated the total concentrations of PCDOs and PCDFs  followed the same
 sequence of abundance by homolog among the facilities.   However,  there
 were no correlations for the individual homologs, or for the relative
 abundances of PCDDs or  PCDFs in the PCDD/PCDF  total  concentrations.
      Upon comparing the field leachate results  with  the results from the
 quench water samples,  the following observation was  noted.   The field
 leachate samples  from Facilities B and C contained more PCDDs  and PCDFs
 than the quench water samples from the facilities.   However, the  quench
 water samples from  Facility D contained 10 times more  PCDDs  and PCDFs
 than the field leachate samples from this facility.  This  suggests that
 the  PCDDs and PCDFs  at  Facility D are readily  leached  from the solid ash
 material  in  the quench  water tank.   Conversely,  at Facilities  B and  C the
 PCDDs  and PCDFs appear  to leach more slowly until the  ash  is disposed in
 the  landfill.
      4.4.4  Organic  Constituents
     The  field  leachates, quench  water,  and ground water samples  were
 analyzed  for  organic constituents,  including:   TOC,  organic scan,  and
 BNAs.  The results of these  analyzes  are  summarized  by  sample  matrix and
 facility  in Table 4.14.
     A review of the field  leachate  data  showed that Facility  D,  had the
 highest TOC and BNA constituent concentrations.   Similarly, Facility B
 had the lowest TOC and BNA constituent concentrations.   The predominant
 BNAs were thiolane, ethylhexyl phthalate,  and dimethylpropanediol.
     A review of the quench water data showed that the  variabilities
between units and facilities were relatively large.  Facility  D had  the
highest concentrations of TOC and BNA constituents,  followed sequentially
                                   4-51

-------
                                 TABLE 4.14  ORGANIC CONSTITUENTS IN  FIELD HATER SAMPLES

FIELD LEACHATES
Sample
Plant Description
a
8
3
C
C
C
0
0
0





East Side
Northeast Corner
North Side
Northwest Corner
Northeast Corner
North Side
Southeast Corner
Northeast Corner
Northeast Corner, Oup
No.
M1n.
Max.
Avg.
Std. Oev.
TOC
(mg/D
189.0
204.0
273.0
379.0
187.0
59.1
574.0
636.0
567.0
9
59.1
636
340.9
195.4
Organic
Scan
0«0/1)
<0.25
<0.25
<0.25
<0.25
2.5
<0.25
<0.25
<0.2S

8
0
2.5
NA
NA
Ethyl Dimethyl
SNA Hexyl Propane Hexa
Peaks Phthalate Dlol Blphenyl Thlepane Thlolane
Found 117817 126307 90437 17233715 289167
(No.) (ug/L) (ug/L) (ug/L) (ug/L) (ug/L)
2
3
4
2
8
1
21
22
24
9
1
24
9.7
9.2




12

7
80
37
4
7
30
34.0
28.9

9
22




110
120
4
9
120
65.3
50.1







51
51
2
51
51
51.0
Q.O







82 400
140
1 2
82 140
32 400
82.0 270.0
0.0 . 130.0
              Sanple
Plant       Description

  B          East Side
  3      Northeast Corner
  3         North Side

  C      Northwest Corner
  C      Northeast Corner
  C         North Side

  0      Southeast Corner
  0      Northeast Corner
  0    Northeast Corner,  Oup

                No.
               Hln.
               Max.
               Avg.
             Std. Oev.
          Sulfo-
  Benz-   nylbls
aldehyde  Sulfur
  100527    67710
 (ug/L)   (ug/L)
       1
       8
       8
     8.0
     0.0
               11
   1
  11
  11
11.0
 0.0
      Unknown
        HCs   Unknowns
        (*)      (#)




2

4
9
10
2
2
3
1
4
1
16
3
10
                                                    4-52

-------
                                 TABLE 4.14  ORGANIC CONSTITUENTS  IN  FIELD HATER  SAMPLES
           QUENCH WATER



Plant
A.
A
B
B
B
• c
C
0
0
0





............

Saujjle
Description
Unit 2. 9/26
Unit 1. 9/26
Unit 3. 9/28
Unit 4, 9/28, Oup
Unit 4. 9/28
Unit 2. 9/28
Unit 2. 9/30
Unit 2, 10/3
Unit 2. 10/3, Oup
Unit 2. 10/4
NO.
M1n.
Max.
Avg.
Std. Dev.


TOC
(*B/1)
94.5
26.9
77.3
421.0
416.5
3.2
29.2
165.0
153.0
1228.0
10
3.2
1228
261.5
352.4

Organic
Scan
(•B/U
<0.25
<0.25
<0.25
<0.25
<0.25
12.3
<0.25
<0.25

<0.25
9
0.125
12.3
1.48
3.33
SNA
Peaks
Found
(No.)
29
8
23
20
20

5
25
25
25
9
5
29
20.0
7.7

Phenol
108952
(ug/L)
65

170
380
380


60
71
640
7
60
640
252.3
205.2
2 -Methyl
phenol
95487
(ug/L)
6

17
40
44


7
7
36
7
6
36
29.6
27.3
4-Methyl Dimethyl Benzole
phenol
106445
(ug/L)



92
94


23


3
23
94
69.7
33.0
phenol Acid
105679 65850
(ug/L) (ug/L)
36
260
300
2100
2100


570
900
44 3800
1 3
44 36
44 3800
44.0 1258.3
. 0.0 1219.0
Naphtha-
lene
91203
(ug/L)
3









1
8
8
8.0
0.0
              Sample
Plant       Description

  A        Unit 2,  9/26
  A        Unit 1,  9/26

  B        Unit 3,  9/28
  8      Unit 4, 9/28,  Dup
  B        Unit 4,  9/28

  C        Unit 2.  9/28
  C        Unit 2.  9/30

  0        Unit 2.  10/3
  0      Unit 2, 10/3,  Dup
  0        Unit 2,  10/4
                                              Ethyl    Methyl
Acenaph- Phenan-   Butyl   Fluor-             Hexyl   Butanoic Molecular
thylene  threne  Phthaiate anthene  Pyrene  Phthalate  Acid    Sulfur  Thiolane
 208968    35013    84742   206440   129000   117817  116530   10544500  289167
 (ug/L)  (ug/L)   (ug/L)   (ug/L)   (ug/L)   (ug/L)    (ug/L)    (ug/L)   (ug/L)
                                                           33
                                                                    29
                                                                   130
23
No.
M1n.
Max.
Avg.
Std. Oev.

1
6
6
6.0
0.0

1
6
6
6.0
0.0

1
3
3
3.0
0.0
4-53
1
6
6
6.0
0.0

1
5
5
5.0
0.0

1
8
8
8.0
0.0

1
33
33
33.0
0.0

2
29
130
79.5
50.5

1
23
23
23.0
0.0


-------
                   TABLE 4.14  ORGANIC CONSTITUENTS  IN FIELD WATER SAMPLES




Plant
A
A
a
8
B
C
C
0
0
0





QUENCH HATER



Sanple
Description
Unit 2. 9/26
Unit 1. 9/26
Unit 3, 9/28
Unit 4, 9/28. Oup
Unit 4, 9/28
Unit 2. 9/28
Unit 2, 9/30
Unit 2. 10/3
Unit 2. 10/3. Oup
Unit 2. 10/4
No.
M1n.
Max.
Avg.
Std. Oev.
2-Hydrox
Benzole
Acid
69727
(ug/L)


40
SO
42





3
40
50
44.0
4.3
Hydroxy
Methyl
Pentenone
80717
(ug/L)


26







1
26
26
26.0
0.0
Pyran Hydroxy
Naphtho Methyl
01 one Pyranone
81845 118718
(ug/L) (ug/L)
6 11








130
1 2
6 11
6 130
6.0 70.5
0.0 59.5

Hydro Hexanoic
Pyranone Add
S42280 142621
(ug/L) (ug/L)
11 22
10
30
58
37


45
51
920
1 8
11 10
11 920
11.0 146.6
0.0 292.7
Methyl
Pentanolc Benz-
Acid aldehyde
646071 100527
(ug/L) (ug/L)







17 22
84
38
3 1
17 22
88 22
63.0 22.0
32.6 0.0
Methyl
Pentane-
diol
144194
(ug/L)







17


1
17
17
17.0
0.0
Sample
Plant
A
A
B
a
8
C
C
0
0
0
Description
Unit
Unit
Unit
Unit 4
Unit
Unit
Unit
Unit
Unit 2
Unit
2. 9/26
1. 9/26
3. 9/28
, 9/28, Oup
4. 9/28
2, 9/28
2. 9/30
2. 10/3
. 10/3. Oup
2. 10/4
                Furan   Benzene   Tetra   Methyl    Benzene
               Carfaox- Propanolc Oecanolc Purlne    Acetic  Oecanolc
               aldehyde  Add     Add     01 one    Acid     Acid    Unknown  Unknown
                 67470   501520   544638    58082  103822   334485 Org Adds   HCs   Unknowns
                (ug/L)  (ug/L)   (ug/L)   (ug/L)    (ug/L)    (ug/L)     (#)      (*)      (I)

                                                                          2                15
                                                                                            6
                                                                                           16
                                                                                           13
                                                                                           12
   No.
  Min.
  Max.
  Avg.
Std. Oev.
54


1
54
54
54.0
0.0

23
12

2
12
23
17.5
5.5

72 23
22

1 2
72 22
72 23
72.0 22.5
0.0 0.5
4-54


120
1
120
120
120.0
0.0



160
1
160
160
160.0
0.0

                                                                                            9
                                                                                           17
                                                                                           13

-------
                                 TABLE 4.14  ORGANIC CONSTITUENTS IN FIELD WATER SAMPLES
            GROUNONATER
 Plant

  A

'  B
Sample
Description
SNA
Organic Peaks
TOC Scan Found
(iag/1) (mg/1) (No.)
#1
#2
3.4    <0.25
2.7    <0.25
                No.
               M1n.
               Max.
               Avg.
               Std.
                   6
                   2
                97.4
               43.75
               41.56
                                         Ethyl
                                         Hexyl
                                       Phthalate
                                         117817 Unknowns
                                        (ug/L)      (I)
c
c
c
c
#3
117
#4
Production Well
80.9
76.1
97.4
2.0
<0.2S
<0.2S
<0.2S
<0.2S
0
2
0

                       NOTE:
                             Names of organic constituents abbreviated:
                             CAS  numbers provided with constituent names
                                                     4-55

-------
 by Facilities B, A, and C.  The predominant BNAs detected w«re benzole
 acid,  phenol, hexanoic acid, benzene acetic acid, and decanoic acid.
     A review of the ground water data showed that the variability of the
 TOG data between facilities was relatively high.  Facility C had the
 highest TOC concentrations, with Facilities A and B having approximately
 equal  concentrations significantly less than Facility C.  Only one ground
 water  sample contained detectable quantities of BNA constituents -
 Well 17 at Facility C.  The only BNA positively identified was
 bis-ethylhexyl phthalata.
     Upon comparing the results from the different sample matrices, the
 following observations were noted.  First, the quench water contained the
 highest quantities of BNA constituents, and the second highest quantity
 of  TOC.  The field leachates contained the highest concentrations of TOC
 and the second highest of BNA constituents.  Second, there appeared to be
 a slight correlation between TOC and BNA concentrations, however, there
 did not appear to be any relationship between TOC or BNA and organic
 scan.    Finally, it was observed that certain BNA compounds were always
 detected together.  Phenol, methylphenol (phenolic derivatives), benzoic
 acid,  and hexanoic acid (carboxylic acids) were always found together, as
 were naphthalene, acenaphthylene, phenanthrene, fluoranthene, and pyrene
 (polycyclic aromatic hydrocarbons).
     4.5  Quality Assurance/Quality Control Summary
     The Versar laboratory and Versar's subcontract laboratory, Battelle.
Columbus, which conducted analyses for PCDDs and PCDFs, implemented
 extensive quality control measures on all analyses.  The procedures used
by  the  Versar laboratory conformed to the EPA Contract Laboratory  Program
 requirement*.  During all analytical activities, quality control  (QC)
 samples were introduced into the sampling scheme in order  to evaluate  the
precision and accuracy of the analytical method.  These QC samples
 included laboratory-prepared QC samples (e.g.,  reagent blanks,  duplicates,
matrix  spikes, surrogate spikes, and check standards) and  "blind"  field
                                   4-56

-------
 duplicates (at a frequency of  25  percent  per  sampling plan
 specifications)/ trip blanks,  and field blanks.  The field duplicate
 samples were indicative  of the precision  of the  entire sampling and
 analysis method.  The results  of  the QA/QC analyses are summarized in  the
 following subsections by major categories of  analyses—total metals.
-PCBs,  PCDD/PCDFs,  and organic  constituents.   The original data reports
 from the laboratories provide  more extensive  QC  data and are included  in
 the appendices of  this report.  All data  quality objectives and control
 procedures were described  in a QA Plan which  was submitted to EPA for
 review and approved prior  to the  initiation of chemical analysis.
     4.5.1  Internal  QA/QC
     The internal  QA/QC  samples were prepared in the laboratory as
 required by the analytical  method to evaluate the performance of the
method.   The  following sections present the results and evaluations of
the internal  QA/QC samples  for metals, PCBs,  PCDD/PCDFs, and organic
constituents.
     4.5.1.1   Total Metals  Analyses - Analyses of solid residues, field
water  samples,  and laboratory-prepared leachates for total metals were
performed by  the Versar  laboratory.  Analyses of each sample batch for
each matrix  (solid, field water,  laboratory leachates) were accompanied
by  internal QC checks  consisting  of the following analyses:  reference
standard,  calibration  blank, one  or two reagent blanks, a check standard
different  from the reference standard, one sample duplicate selected at
random from the batch, and  one spike.  The standards were used to check
on  the accuracy of calibration, the blanks are used to identify
contamination  in reagents and  laboratory  water,  the duplicates indicate
the precision or reproducibility  of the analyses as the Relative Percent
Difference (RPD), and  the spikes  indicate the accuracy of analyses in
terms of the capabilities of the  analyses to  measure the constituent,  or
percent recovery of any added spike.
     The results of these internal QC cheeks  for total metal analyses  are
summarized in Table 4.15.  The QC criteria for total metals analyses  in
                                   4-57

-------
                                      TABLE 4.15  QC SUMMARY (INTERNAL) FOR METALS
                                                          ICP ANALYSES
                                                                       AA ANALYSES
t ly Asn ana BOTIOM *sn
Olgestates
Reference Standard
Calibration Blank
Reagent Blank 1
Reagent Blank 2
Check Standard
Sanple Duplicate
(Sanple 17667)
Spike Recovery
Field water Saoples
(Ground Water a* Quench)
Reference Standard
Calibration Blank
Reagent Blank 1
Check Standard
Sanple Duplicate
(Sanple 19582)
Spike Recovery
Field water Samples
(GW & Field leachates)
UNITS
% Recovered
ug/L
ug/L
ug/L
* Recovered
%RPO

% Recovered
Cd
97.1
*10
*10
<10
95.7
4.3

(2)
Cr
97.4
<5
<5
<5
91.7
0.0

20.0
Cu
98.0
<5
<5
<5
92.5
5.2

(2)
Fe
103.1
<4
13
20
97.4
15.1

(2)
Pb
101.6
<50
<50
<50
93.3
4.4

(2)
Nn
95.7
<2
2.1
«2
91.4
4.6

(2)
Nt
92.9
<15
<15
<15
95.3
1.4

(2)
Zn
97.7
<3
4.2
9.5
95.0
3.9

(2)
ICP ANALYSES
UNITS
% Recovered
ug/L
ug/L
* Recovered
WPO

% Recovered
Cd
98.6
<10
<10
101.7
0.0

32.0
Cr
94.4
<5
8.9
98.0
(1)

35.1
Cu
95.5
<5
5.5
100.0
1.1

39.0
Fe
95.5
<4
27
98.5
67.7

36.3
Pb
98.6
<50
<50
98.4
(I)

79.5
Nn
95.0
<2
19
98.5
5.6

91.5
HI
96.0
<15
<15
102.0
(1)

33.5
Zn
99.5
«3
9.3
104.5
13.3

36.0
ICP ANALYSES
UNITS
Cd
Cr
Cu
Fe
Pb
Hn
N1
Zn
As
100.0
*10
<10

114.0
18.0

(2)
Se Hg
39.6 93.2
<5 <0.2
<5 <0.2

38.0 108.0
3.3 (I)

50.0 98.0
AA ANALYSES
AS
104.3
<10
<10
91.0
(1)

104.0
AA
AS
Se Hg
37.6 102.3
<5 <0.2
<5 <0.2
100.0 38.0
(1) (11

36.0 115.0
ANALYSES
Se Hg
Reference Standard
Calibration Blank
Reagent Blank 1
Check Standard
Saople Duplicate
    (Sanple 19765)
Spike Recovery
* Recover*    98.2   94.8   93.5   93.5  103.6   94.0   95.0   99.5  106.5   35.7   97.7
    ug/L       <10    <5     <5     «5     <50    <1     <15      13   <10    <5     «0,I
    ug/L       <10    <5       44     21   <50    
-------
                                      TABLE 4.15  QC SUMMARY (INTERNAL) FOR METALS
Field Hater Samples
     Batches 6
 (Field Leachates)
                           UNITS
               Cd
                                       Cr
              Cu
ICP ANALYSES

  Fe     Pb
                     Hn
N1
Zn
 AA ANALYSES

As     Se     Hg
 Reference  Standard
 Calibration  Blank
 Reagent Blank  1
 Check  Standard
 Sample Duplicate
     (Sample  19831)
 Spike  Recovery
% Recovered    97.4   96.3  100.0   98.0  108.1   98.5  106.0   100.5   115.2   37.S   97.7
    ug/L       <10    <5     <5     <5     <50    
-------
                                      TABLE 4.15  QC SUMtARY  (INTERNAL) FOR METALS
SW - 924
1 extract 1 on n
Leachates
ICP ANALYSES AA ANALYSES
UNITS Cd Cr Cu Fe Pb Hn N1 Zn As Se Hg
Reference Standard
Calibration Blank
Reagent Blank 1
Reagent Blank 2
Check Standard
Sample Duplicate
    (Sample 19517}
Spike Recovery
% Recovered    99.4   97.2   98.5   95.0   96.4   96.0   98.0   97.5  104.3   87.6   97.7
    ug/L       <10    <5     <5     <5     <50    
-------
 the project were an RPD between duplicate analyses of 0-20 percent, and
 an accuracy (t recovery of spikes) of 75 to 125 percent in conformance to
 the EPA Contract Laboratory Program.
     No significant problems were encountered in maintaining calibration
 or with contamination of reagents or laboratory water.  Occasionally ,
 some metals ware detected in calibration and reagent blanks in the low
 microgram per liter (ug/L) range.  Normally, no corrections of the sample
 analytical results for the blanks w«re required.
     The precision criteria (RPD on duplicates) were generally achieved
 with some exceptions.  In the analyses of field water samples, Fe
 exceeded the criteria in analysis of Batches 1-4, Zn exceeded the
 criteria in analysis of Batch 5, and Cu and Mn exceeded the criteria in
 analysis of Batch 6.  In the analyses of laboratory-prepared leachates,
 the Versar laboratory encountered difficulty in achieving the criteria in
 analyses for Cd, Cr, Cu, Fe and Ni in the EP leachate, Cd, Fe, Pb, Mn, Ni
 and Zn in the TCLP leachate, and Mn, Zn, and Se in the first extract by  -
 the MWEP.   The problems with the analysis of laboratory leachates may
 have been related to the relatively low concentration levels for some of
            •
 these metals in 'the leachates and the inherent increased variability at
 these low levels.
     The accuracy criteria (% recovery of spikes) were also generally
achieved with few exceptions.  In the analysis of the solid residue
digestates, the criteria for Cr was below the lower limit.  In the
analyses of field water samples, the criteria for Pb was below the lower
 limit in Batch 5, and the criteria for Cu and Pb were below the lower
 limit in Batch 6.  In the analyses of the laboratory-prepared leachates,
the criteria for Ni was below the lower limit in the EP leachates  and  the
TCLP leachates, the criteria for Cu, Zn and Se were below the criteria in
the first extract by the MWEP, and the criteria for Hg was slightly above
the upper limit in the second extract by the MWEP.
     Overall,  however, the analyses for total metals  in all matrices  were
in control.  The data from the analyses of samples are, therefore.
                                   4-61

-------
 considered valid.   Corrective actions were taken by the laboratory on
 each occasion of a criteria exceedance  in accordance with the Quality
 Assurance Project  Plan.  These corrective actions maintained control in
 the total metals analyses.
      4.5.1.2   Polychlorinated Biphenyls - Analyses of solid residues and
 selected field water  samples for polychlorinated biphenyls (PCBs) were
 conducted by  the Versar  laboratory.  Samples were analyzed in three
 separate groups  at different times.  The first group of samples consisted
 of  all  fly ash samples collected at the four facilities.  The second
 group of samples consisted of selected field water samples including
 quench  water,  leachates  collected at the monofilled landfills, and ground
 water.   The third  group  of samples consisted of other ash samples
 including bottom and  combined bottom/fly ash, size fractions of fly ash
 samples  collected  at  Facility C, and composite samples collected from the
 monofilled landfill at Facilities C and D.  Analyses of each group
 (except  as  noted below)  were accompanied by internal QC checks consisting
 of  the  following:   (1) analysis of reagent blanks', (2) determination of
 the recoveries of  four isotopically-labeled (carbon  ) isomers added as
 surrogate  spikes to all  samples prior to extraction to track the
 performance of the extraction, cleanup, and analysis of each sample, and
 (3) determination of  the recoveries of matrix spike (MS) and matrix spike
 duplicates  (MSD) on two  field water samples.  The MS and MSD consists of
 a mixture of Arochlors 1016 and 1260 and are used to determine accuracy
and precision.  No criteria for the recovery of surrogate spikes or for
the relative percent  difference (RPO) between the matrix spikes and
matrix spike duplicates have been established for this method.
     The results of these internal QC checks for the PCS analyses are
 summarized  in Table 4.16 and are discussed below.
     No PCBs were detected in any of the laboratory reagent blanks
accompanying each group of samples analyzed, indicating that the
 laboratory water and  reagents were free of PCS contamination.
                                   4-62

-------
TABLE 4.16  QC SUMMARY (INTERNAL) FOR PCB ANALYSIS
           Surrogate Recovery (%)

Facility
A
A
A
A
A
A
A
A
A
A
A
A
A
A
a
3
B
3
3
3
3
a
3
a
a
a
3
8
B
a
a
a
a
a .
Sa*>le
Matrix
Fly
Fly
Fly
Fly
Fly
Bottom/Fly
8ottOfll/Fly
3ottoa/Fly
Bottom/Fly
Bottom/Fly
Bottoa/Fly
Bottoa/Fly
Quench
Quench
Fly
Fly
Fly
Fly
Fly
Fly
Fly
Bottom
Botto»
Botton
8otto»
Bottom
Quench
Quench
Quench
Hacftate
leachate
leachate
LMChate
Letchate
Sample
Description
Unit 1, 9/26, AN
Unit 1. 9/26. AM, Oup
Unit 1. 9/26, PM
Unit 2. 9/26, AM
Unit 2, 9/26, PM
Unit 1. 9/26, AM
Unit 1, 9/26, PM
Unit 1. 9/26. PM
Unit 1, 9/26, PN
Unit 2, 9/26, AM
Unit 2, 9/26, AM, Oup
Unit 2. 9/26, PM
Unit 1. 9/26
Unit 2. 9/26
Unit 3, 9/28, AM
Unit 3, 9/28. AM, Oup
Unit 3, 9/29, PM
Unit 4, 9/28, AM
Unit 4. 9/29, PM
Unit 4, 9/29. PM
Unit 4, 9/29, PM
Unit 3. 9/28. AM
Unit 3, 9/29, PM
Unit 4. 9/28. AM
Unit 4, 9/28, AM, Oup
Unit 4. 9/29, PM
Unit 3. 9/28
Unit 4, 9/28
Unit 4. 9/28. Oup
East Side
North Side
Northeast Corner
Northeast Corner
Northeast Corner
Sanple
Nutter
17628
17631
17637
17643
17646
17625
17640
17640MS
17640MSO
17619
17622
17634
17546-47
17556-57
17669
17672
17693
17680
17686
17686MSO'
17686MS
17666
17690
17674
17677
17683
17596-97
17606-47
17536-37
19837-38
19859-60
19846-47MSO
19846-47MS
19846-47
4-Chloro-
Biphenyl
3
0
0
9
1
51
64
57
48
54
66
67
74
52
0
0
3
0
0
3
0.3
59
65
34
60
71
56
74
98
59
66
54
56
55
                                   3,3'.4,4'    Octa
                                  Tetrachloro  Chloro
                                   Blphenyl   Blphenyl
                                       0
                                      1.4
                                       4
                                       9
                                       0
                                      69
                                      105
                                      94
                                      75
                                      68
                                      76
                                      32
                                      90
                                      71

                                       0
                                       0
                                       1
                                      0.3
                                       0
                                       3
                                       0
                                      34
                                      76
                                      48
                                      75
                                      78
                                      71
                                      94
                                      111
                                      34
                                      98
                                      71
                                      87
                                      33
87
80
74
29
68
73
107
94
75
66
70
74
78
65

78
60
32
68
15
85
58
93
106
69
92
101
60
113
139
78
87
60
69
58
  Oca
 Chloro
Blphenyl

   95
   108
   33
   33
   30
   72
   78
   90
   65
   55
   59
   56
   79
   67

   77
   49
   32
   72
   17
   36
   74
   72
   104
   67
   87
   82
   66
   129
   165
   33
   83
   60
   42
   52
               4-63

-------
                                TABLE 4.16  QC SUMMARY (INTERNM.) FOR PCS ANALYSIS
                                           Surrogate Rtcovtry (continued)
           SaapU
Facility   Matrix
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c
c

0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
            Fly
            Fly
            Fly
            Fly
            Fly
            Fly
            Fly
            Fly
         8ottoa/Fly
         Bottom/Fly
         Bottom/Fly
         Bottom/Fly
         Bottom/Fly
          Landfill
          Leachate
          Leachate
          Leacnate
           HWell
  HWeU
  MWell
  Well
  Pwell
  Quench
  Quench

   Fly
   Fly
   Fly
   Fly
   My
BottoeVFly
BottOB/Fly
aottoiYFly
Bottom/Fly
BottoeVFly
BottOB/Fly
Bottoa/Fly
 Landfill
 Leachate
 Leachate
 Leachate
  Quench
  Quench
  Quench
                   Saeple
                 Otscrlption

              Unit 2.  9/28.  PN
              Unit 2,  9/29,  PM
            Unit 2. 9/29,  PH,  Oup
              Unit 2.  9/30,  AM
              Unit 2.  9/30,  PN
               Unit 2, Coarse
             Unit 2. Fine (ESP)
               Unit 2, HedluB
              Unit 2,  9/28.  PH
              Unit 2,  9/29,  PH
              Unit 2.  9/30.  AM
            Unit 2, 9/30,  AM,  Oup
              Unit 2.  9/30.  PH
             Perimeter Conpos Itt
                 North Side
              Northtast Corner
              Northeast Corner
                    117
                              #3
                              *4
                        Production Mil
                         Unit 2. 9/28
                         Unit 2. 9/30

                      Unit 1-2. 10/3. AM
                    Unit 1-2. 10/3, AM.  Oup
                      Unit 1-2. 10/3. PH
                      Unit 1-2. 10/4, AN
                      Unit 1-2. 10/4. PN
                      Unit 1-2. 10/3, AN
                      Unit 1-2. 10/3. PN
                      Unit 1-2. 10/3. PN
                      Unit 1-2. 10/3. PN
                      Unit 1-2. 10/4. AN
                    Unit 1-2. 10/4. AN.  Oup
                      Unit 1-2. 10/4, PN
                      Perimeter Composite
                       Northeast Corner
                       Northeast Corner
                       Southeast Corner
                         Unit 2. 10/3
                       Unit 2, 10/3, Oup
                         Unit 2. 10/4

Saople
Muter
19519
19543
19546
19585
19598
19549
19555
19552
19515
19540
19588
19590
19595
19523
19805-06
19793-94
19817-18
19785-36MSO
19785-86
19785-86W
19759-40
19772-73
19579-80
19509-10
195M-«7
19669
i 19672
19681
19687
19708
19677
19684HSO
196B4NS
19664
19690
t 19693
19712
19600
19623-24
19636-37
19610-11
19649-50
19662-13
19703,27
4-64

4-Chloro-
Blphtnyl
32
98
40
52
112
0.2
11
41
86
51
70
60
10
267
68
59
32
106
63
98
64
58
72
130
62
44
43
14
53
23
40
64
66
61
1
54
59
59
52
48
64
50
SO
42

3,3' .4,1
Tttrachli
Blphtny
42
76
51
64
121
0
9
70
81
75
34
87
21
159
91
109
33
113
103
116
115
102
113
180
85
36
27
7
50
20
94
104
94
90
99
113
87
86
101
90
75
81
102
57

  Octa
 Chloro
Blphenyl

   32
   128
   96
   77
   129
   32
   76
   96
   100
   33
   79
   37
   23
   111
   82
   107
   30
   105
   114
   103
   97
   96
   132
   170
   36

   80
  .138
   97
   104
   73
   102
   105
   102
   39
   36
   99
   78
   80
   114
   95
   30
   65
    92
    60
  Otca
 Chloro
Blphenyl

   63
   109
   34
   37
   35
   74
   30
   87
   87
   38
   35
   79
   21
   45
   38
   37
   26
   31
   109
   35
   77
   78
   120
   107
   105

   92
   156
   124
   97
   75
   76
   36
   36
   98
   66
   66
   58
   61
    93
    51
   36
    62
    10S
    39

-------
                             TABLE 4.16  QC SUMMARY (INTERfML) FOR PCB ANALYSIS
                                        Surrogate Recovery (continued)

Sanple
Matrix
Blank
Blank
Blank
Blank
Blank
Blank

Saaple
Description
Laboratory
Laboratory
Laboratory
Laboratory
Laboratory
Laboratory

Sa^lt
Nwber
RM310
RMS76
RB*S78
RBM17
RW633
RM635

4-CJiloro-
Blphenyl
50
42
31
21
59
54
3,3',4,4'
Octa
Tetrachloro Chloro
Biphenyl
61
76
86
93
88
92
Biphenyl
56
90
97
96
99
93
Oeca
Oiloro
Biphenyl
36
34
96
103
33
36
                                        Matrix Spike Results for PCB Analyses
B      Leacnate     Northeast Corner      19846-47
C       MWell              117            19785-66
A     Bottom/Fly    Unit 1. 9/26. PM         17640
0     Bottom/Fly   Unit 1-2, 10/3, PM        19684
MS

45
75
USD

42
78
RPO

 2
 3
                                            4-65

-------
     The Vtrsar laboratory experienced significant difficulties with the
analysts of the first group of samples consisting of 20 fly ash samples.
The problems are summarized in Section 3.4.2 of this report and detailed
in the data appendices.  The problems are reflected in poor recoveries of
the lower molecular weight surrogate spikes (4-chlorobiphenyl and
3,3',4,4" tetrachlorobiphenyl) from the fly ash samples collected at
Facilities A and 3.  After some adjustments to the procedures for cleanup
of the extracts, recoveries of these surrogate spikes were improved as is
reflected in the recoveries from the fly ash samples collected at
Facilities C and 0.  However, the problems with poor recoveries of the
lower molecular weight surrogate spikes recurred in some of the bottom
and combined bottom/fly ash samples analyzed in Group 3.  The recoveries
of the higher molecular weight (octachloro and decachloro biphenyls)
surrogate spikes were consistently better than those for the lower
molecular weight surrogate spikes in the fly ash samples.  Recoveries
ranged from 15 percent to 135 percent for octachloro biphenyl and
17 percent to 156 percent for decachloro biphenyl.
     Recoveries of all surrogate spikes from the field water samples
(analyzed as Group 2) were good; ranges are as follows:  4-chlorobiphenyl,
32 percent to 130 percent; tetrachloro biphenyl, 33 percent to
130 percent; octachloro biphenyl, 30 percent to 139 percent; decachloro
biphenyl, 26 percent to 120 percent.
     The Versar laboratory again experienced some problems with recoveries
of the lower molecular1 weight surrogate spikes in the analyses of the
other ash samples (Group 3).  The recoveries of 4-chloro biphenyl were
10 percent or less for three samples, and the recoveries of tetrachloro
biphenyl were 10 percent or less for two samples.  The poor recoveries
were largely associated with analyses of the coarse and fine fly ash
samples from Facility C.  With these exceptions, however,  recoveries  were
good,  with ranges as follows:  4-chloro biphenyl, 11 percent to
267 percent; tetrachloro biphenyl, 21 percent to 159 percent;  octachloro
biphenyl, 23 percent to 111 percent; decachloro biphenyl,  21 percent  to
                                   4-66

-------
 104 percent.  The poor recoveries  for some  QC  samples may be related  to
 the strong attractive force which  causes  the PCBs  to be absorbed onto the
 surface of the solid substrates  (i.e.,  fly  ash particles).
      The recoveries of matrix  spikes  and  matrix  spike duplicates using a
 SO/SO mixture of native Arochlor 1016 and 1260 as  the spikes were
 determined on two field water  samples.  Due to the problems encountered
 initially in the analyses  of the fly  ash  samples (Group 1) matrix  spikes,
 no duplicates were analyzed for  the ash samples.
      The recoveries on the matrix  spikes  (MS)  and  matrix spike duplicates
 (MSD),  and the relative percent  difference  (RPD) between the two spikes
 were  excellent for the liquid  samples indicating good precision in the
 analyses.   The recoveries  of the matrix spikes of  the ash samples  were
 51 percent/  100 percent, and 92  percent.
      The analyses  of PCB homologs  in  fly  ash samples (Group I), field
 water samples (Group 2), and other ash samples (Group 3) overall were in
 control, with one  exception.   The  analyses  for the lower molecular weight
                                                        *
 PCB home-logs  (tetrachloro  biphenyls)  in the fly  ash samples from
 Facilities A  and B (analyzed in  Group 1)  were  not  in control.  The
 results  of analyses for the  lower  molecular weight PCB hooologs in these
 samples  are probably biased  toward low  values  due  to poor surrogate spike
 recoveries.   The results of  analyses  for  the higher molecular weight  PCB
 homologs (pentachloro biphenyls  and more  chlorinated) in all samples  are
 probably as accurate a* current  methodology is capable of achieving.   The
                         •    «
 results  of analyses for the  lower  molecular weight PCB hooologs
 (tetrachloro  biphenyl and  lighter) in all samples  except the fly ash
 samples  from  Facilities A  and  B  are accurate for the intended use  of  the
 data.
      4.5.1.3   PCDD/PCDFs - Analyses for solid  residues, selected field
water samples, and  TCLP leachates  of  selected  solid residue samples for
PCDDs and PCDFs were  performed by  Versar's  subcontract laboratory,
Battelle, Columbus.   Analyses  of each batch of samples for each matrix
                                   4-67

-------
 were accompanied by internal QC checks consisting of the following:
 analysis of method blanks, determination of recoveries of five
 isotopically-labeled PCDO and four isotopically-labeled PCOF internal
 standards added to each sample, blank and native spike sample prior to
 extraction and analyses, and determination of recoveries of native
 PCDD/PCDF spikes in 1 sample per batch (frequency of S percent).  The
 results of the recovery of the nine isotopically labeled internal
 standards are presented in Table 4.17.
     Native spike and laboratory method blank samples were processed
 during the extraction and cleanup of the samples.  The native spike
 sample was used to evaluate accuracy, while the laboratory method blank
 samples were used to demonstrate the absence of contamination.
     The samples were analyzed in three batches.  The first batch
consisted of 20 fly ash samples from the four facilities.  The second
batch consisted of bottom ash or combined bottom/fly ash from the four
facilities, composites of sample collected from the perimeter of
landfills at Facilities C and 0, and coarse and.fine fractions of a fly
ash sample from Facility C.  The third batch consisted of field waters
(field leachate and quench water samples) and leachates prepared in the
laboratory by the TCLP method using selected samples of fly ash and
bottom ash, or combined bottom/fly ash from the four facilities.
     In the first batch of 20 fly ash samples, the method blank analyses
were free of PCDD/PCDF contamination, except for trace levels of
hepta-CDD and octa-CDD.  The observed levels were less than the desired
detection limit for these congener classes and should, therefore, not
adversely affect the analytical results.  Recovery of the analytes from
the native spike sample* ranged from 90 to 110 percent, which is within
the expected range of variation, and within the QC criteria specified  in
the Quality Assurance Project Plan (QAPP).
     The recoveries of the nine isotopically-labeled internal standards
in fly ash samples were used to correct analytical results for  extraction
                                   4-68

-------
TABLE 4.17  QC SIMMRY (INTERNAL) FOR PCOO/PCOF ANALYSIS
          Internal Standard (%) Recovery


Facility
A
A
A
A
A
A
A
A
A
A
A
A
A
3
8
a
a
a
a
a
a
a
a
a
a
a
a
a
a
3

Sanple
Matrix
Fly Ash
Fly Ash
Fly Ash
Fly Ash
Fly ASh
Bottom/Fly
Bottom/Fly
Sot torn/Fly
Bottom/Fly
Bottom/Fly
Fly Ash
Quench
Quench
Fly
Fly
Fly
Fly
Fly
Bottom
Bottom
Bottom
Bottom
Bottom
Bottom Ash
Fly Ash
leachatt
Leachate
Leacnate
Quench
Quench

Sample
Description
Unit 1. 9/26. AN
Unit 1. 9/26. AN, Oup
Unit 1. 9/26. PH
Unit 2. 9/26. AN
Unit 2. 9/26, PH
Unit 2. 9/26. AN
Unit 1. 9/26, AN
Unit 2, 9/26, PN
Unit 2. 9/26, AN
Unit 2. 9/26. AN
Lao Leacnate (TCLP)
Unit 2. 9/26
Unit 1. 9/26
Unit 3. 9/28. AN
Unit 3. 9/28. AN, Oup
Unit 4, 9/28, AN
Unit 4. 9/29. P*
Unit 3. 9/29, PN
Unit 4, 9/28, AN
Unit 4, 9/28. AN. Oup
Unit 3, 9/28, AN
Unit 4. 9/29. PN
Unit 3. 9/29, PN
Lab Leacnate (TO?)
Lab Leacnate (TOP)
North Side
Northeast Corner
East Side
Unit 4, 9/28, Oup
Unit 4. 9/28
PCOO/

PCDf TETRA
No.
17629
17632
17638
17644
17647
17620
17624
17635
17620
17620,
17844
17552-5
17542-4
17668
17671
17681
17687
17692
17675
17678
17665
17684
17689
17675
17681
198*5-6
19852-5
19639-4
17532-3
17602-0
-COO
39
92
74
120
34
32
34
89
32
110
94
97
98
83
39
71
85
98
72
92
39
52
92
99
93
33
89
92
70
92

PENTA
-COO
81
80
79
125
61
99
76
100
27
110
110
100
97
55
74
75
75
115
82
82
83
96
88
94
98
37
87 "
102
71
110

HEXA
-COO
57
58
59
85
46
95
71
99
34
93
39
110
100
50
62
58
56
53
74
74
78
94
36
85
100
30
72
95
60
110

HEPTA
-COO
74
76
67
94
44
98
64
98
36
110
86
120
100
50
66
69
43
30
. 72
67
75
91
84
95
110
30
70
100
57
120

OCTA
-COO
76
72
63
93
37
100
61
99
40
120
87
130
110
41
56
77
20
43
65
61
71
96
80
104
120
30
71
109
58
130

TETRA
-CDF
85
94
36
154
85
32
35
99
32
110
94
100
99
95
100
88
38
109
69
37
38
44
91
90
96
31
90
94
70
89

PENTA
-CDF
89
90
86
128
70
90
79
98
31
100
100
110
100
73
37
72
78
109
75
79
79
77
86
90
104
33
90
92
64
100

HEXA
-CDF
15
24
22
5
45
33
66
35
31
100
92
96
100
48
64
61
. 54
11
67
65
69
37
74
91
99
31
74
97
60
110

HEPTA
-CDF
1
2
1

4
3
6
3
3i
Hi
9;
• Ui
Hi
4i
6,
4.
4-
s;
6'
6
5J
3,
r.
*
IK
3J
7(
1*
S'
I2i
                      4-69

-------
TABLE 4.17  QC SUMMARY  (INTERNAL) FOR PCOO/PCDF ANALYSIS
          Internal  Standard Recovery (continued)


Facility
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
C
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0

Sample
Matrix
Fly
Fly
Fly
Fly
Fly
Bottom/Fly
Bottom/Fly
Bottoo/Fly
Bottom/Fly
Bottom/Fly
Fly
Fly
Landfill
Landfill
Bottom/Fly
Fly Ash
Leachate
Leachate
Leachate
Quench
Quench
Fly
Fly
Fly
Fly
Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Landfill
SottotVFly
Fly Ash
Ltacnate
Leachate
Quench
Quench
Quench

Sample
Description
Unit 2, 9/28, PN
Unit 2. 9/29, PN
Unit 2. 9/29. PN. Oup
Unit 2. 9/30, AN
Unit 2, 9/30, PN
Unit 2, 9/30. PN
Unit 2. 9/30, AH, Oup
Unit 2. 9/28, PN
Unit 2. 9/29, PN
Unit 2. 9/30. AN
Unit 2. coarse
Unit 2. fine (ESP)
Perimeter Composite (M)
Perimeter Composite (N)
Lab Leachate (TCLP)
Lab Leachate (TCLP)
North Side
Northeast Corner
Northwest Corner
Unit 2. 9/30
Unit 2. 9/28
Unit 1-2. 10/3. AN
Unit 1-2. 10/3. AN. Oup
Unit 1-2. 10/3, PN
Unit 1-2. 10/4. AN
Unit 1-2. 10/4. PN
Unit 1-2. 10/4. AN
Unit 1-2, 10/4. PN
Unit 1-2. 10/3. AN
Unit 1-2. 10/3. PN
Perimeter Composite (H)
Lab Leachate (TOP)
Lab Leecnit* (TCLP)
Northeast Comer
Northeast Corner
Unit 2. 10/3. Oup
Unit 2. 10/4
Unit 2. 10/3
POM/

PCOF TETRA
No.
19520
19544
19547
19584
19597
19594
19590
19516
19541
19587
19550
19556
19524
19524
19541
19550
19807-1
19799-0
19819-2
19562-6
19505-0
19668
19671
19680
19686
19707 "
19689
19711
19676
19683
19601
19676
19668
19632-3
19619-2
19657-6
19698-0
19644-4
-COO
90
100
96
35
113
63
78
78
74
35
47
62
110
90
98
100
97
91
83
100
91
95
90
75
93
97
91
88
86
68
83
100
110
94
96
95
111
64

PENTA
-COO
89
79
94
132
78
73
92
80
75
72
57
30
94
62
86
110
110
31
120
130
110
60
74
95
109
101
92
81
83
75
78
120
97
99
89
94
114
63

HEXA
-ax
35
25
50
107
30
75
80
72
73
66
45
18
33
77
76
97
79
55
100
100
78
30
29
77
54
87
77
78
77
70
73
96
100
70
69
78
82
48

HEPTA
-COO
95
132
102
106
113
60
87
66
66
67
29
26
68
67
75
97
76
47
100
100
30
37
83
91
106
101
77
78
80
69
69
92
98
63
59
80
72
44

OCTA
-COO
65
126
57
51
24
56
34
58
67
62
15
20
58
65
82
98
32
43
120
120
76
106
91
101
109
129
80
80
78
61
68
96
100
59
56
84
64
43

TETRA
-CDF
108
101
97
102
119
68
78
71
75
72
38
56
100
35
91
100
39
93
83
94
39
95
95
90
98
94
88
39
35
68
31
100
99
99
100
95
88
68

PENTA
-COF
34
71
95
125
78
75
33
77
73
65
45
30
95
60
89
100
39
73
93
110
95
59
71
99
106
98
91
80
78
71
75
110
110
92
89
39
99
64

HEXA
-CDF
20
14
5
30
7
71
74
54
45
56
48
13
73
63
73
93
31
56
100
96
33
7
17
24
11
31
78
65
70
65
62
100
98
65
68
78
76
49
                                                                                   /
                                                                                   £
                                                                                   £
                                                                                   C

                                                                                   2
                                                                                   e
                                                                                   6

                                                                                  1C
                                                                                   7

                                                                                  il
                                                                                  1C
                                                                                   a
                     4-70

-------
                                 TABLE  4.17  QC SWHARY (INTERNAL) FOR PCDO/POJF ANALYSIS
                                           Internal Standard Recovery (continued)
           Sanple
Facility   Matrix

           blank
           blank
           spike
           spike

           blank
           blank
           blank
           blank
           blank
           blank
           blank
           spike
           spike
           spike
           spike

           blank
           blank
           blank
           blank
           blank
           spike
           spike
           spike
          blank
       Sample
     Description

    Laboratory *l
    Laboratory 12
Native Laboratory »1
Native Laboratory 12
   Method
   Method
   Method
   Method
   Method
   Method
   Method
   Native
   Native
   Native
   Native
8lank #1
Blank »2
Blank 13
Blank M
Blank *5
Blank #6
Blank #7
Spike #1
Spike tl
Spike n
Spike M
  Method  Blank  »la
  Method  Blank  *2a
  Method  Blank  «a
  Method  Blank  Ma
  Method  Blank  »5a
  Native  Spike  #la
  Native  Spike  «a
  Native  Spike  »3a
     TO? Blank
PCDO/
PCDF TETRA
No. -COO
84
97
95
95
84
90
32
88
76
77
70
66
92
56
74
92
90
93
100
110
88
100
100
75

PENTA
•COO
65
32
72
109
97
100
110
83
81
86
57
70
95
65
91
110
100
100
110
69
100
110
91
80

HEXA
-COO
52
85
49
93
90
78
95
85
75
88
74
67
38
56
91
92
91
99
39
100
35
100
91
63

HEPTA
-COO
54
96
58
102
88
79
39
90
70
81
76
68
98
60
87
92
92
99
37
110
82
110
97
62

OCTA
-030
57
114
62
120
83
31
100
38
74
77
75
69
97
63
88
94
100
94.
91
130
86
120
110
67

TETRA
-CDF
77
102
S3
38
31
91
95
90
73
77
67
65
92
55
51
96
39
91
99
100
39
97
96
66

PENTA
-COF
63
96
72
108
36
32
99
35
69
32
71
65
39
53
79
100
100
95
100
97
91
110
100
69

HEXA
-CDF
47
43
13
30
36
76
95
79
67
32
64
61
30
52
83
92
92
99
36
100
36
100
38
61
                                                     4-71

-------
 efficiancy and cleanup losses.  The expected range of recoveries and QC
 criteria for recovery of the internal standards is 60 to 90 percent.  The
 actual ranges of recoveries for the 20 fly ash samples plus two method
 blanks and two native spike samples is summarized below.

                        RECOVERY RANGE       NUMBER OF OUTSIDE QC CRITERIA
INTERNAL STANDARD
Tetra-CDD-13C12
Penta-CDD-13C!2
Hexa-CDD-13Ci2
Hepta-CDD-13C12
Octa-CDD-13Ci2
Tetra-CDF-13Ci2
Penta-CDF-13C]>2
Hexa-CDF-13Ci2
Hepta-CDF-13Ci2

71
32
25
43
20
77
59
5
5
%
- 120
- 132
- 107
- 132
- 129
- 154
- 128
- 80
- 86
Above
12
3
2
11
9
15-
9
0
0
Below
0
2
17
5
9
0
1
21
19
Total
12
10
19
16
17
15
10
21
19
      The narrow range of expected recoveries of the internal standards
{60 to 90 percent) is typical of samples with relatively clean matrices
and was not often achievable in the analyses of the fly ash samples.
Because the internal standards are used to correct analytical results for
extraction efficiency and cleanup losses, however, the failure to meet
the QC criteria does not affect the quality of the data provided.
      In the second batch of samples consisting of bottom ash, combined
bottom/fly ash, and landfill composite samples, the method blank analyses
were free of PCDD/PCDP contamination except for trace levels of
octa-CDD.  The observed levels were less than the desired detection
limits for these congener classes and should, therefore, not adversely
affect the analytical results.  Recovery of the analytes from the native
spike samples ranged from 90 to 110 percent, which is within the expected
range of variation, and within the QC criteria specified in the QAPP for
this project.

                                   4-72

-------
       As with all analyses,  the recoveries of  the nine  isotopically
 labeled internal standards in these samples were used to correct
 analytical results for extraction efficiency and cleanup losses.   The
 expected range of recoveries and QC criteria for recoveries  is  60  to
 90 percent.   The actual ranges of recoveries for the  22  samples in this
 batch, plus  seven method blanks and four native  spike samples is
 summarized below.

                         RECOVERY RANGE      NUMBER OF OUTSIDE  PC  CRITERIA
INTERNAL STANDARD
Tetra-CDD-13C12
Penta-CDD-13Ci2
Hexa-CDD-13C12
Hepta-CDD-13Ci2
Octa-CDD-l3C12
Tetra-CDF-13Ci2
Penta-CDF-l3C12
Hexa-CDF-13Ci2
Hepta-CDF-l3C12

47
30
13
26
15
38
30
13
20
\
- 110
- 110
- 99
- 98 '
- 100
- 100
- 99
- 95
- 94
Above
5
11
5
4
5
6
. 4
1
1
Below
3
3
3
2
5
5
3
5
5
Total
3
14
3
6
10
11
7
6
6
The recoveries of internal standards from the coarse and fine fractions of
fly ash from Facility C were consistently below the QC criteria, as were
the recoveries from native spike 3.  The recoveries of internal standards
from the remaining samples were generally within or above the QC criteria.
Because the internal standards are used to correct analytical results  for
extraction efficiency and cleanup losses, however, the failure to meet the
QC criteria does not affect the quality of the data provided.
     In the third batch of samples consisting of field waters and
laboratory prepared leachates, the method blank analyses were free of
PCDD/PCDF contamination except for trace levels of octa-CDD.  The
observed levels were less than the desired detection limits for these
congener classes and should, therefore, not adversely affect the
                                   4-73

-------
 analytical  results.  Recovery of the analytes from the native spike
 samples  ranged from 90 to 100 percent, which is within the expected range
 of  variation, and within the QC criteria specified in the QAPP for this
 project.
     As  with all analyses, the recoveries of the nine isotopically
 labeled  internal standards in these samples were used to correct
 analytical  results for extraction efficiency and cleanup losses.  The
 expected range of recoveries is 60 to 90 percent.  The actual range of
 recoveries  for the 26 field waters and laboratory prepared leachates plus
 five method blanks, three native spike samples, and one TCLP blank is
 summarized below.

                        RECOVERY RANGE       NUMBER OF OUTSIDE QC CRITERIA
INTERNAL STANDARD
Tetra-CDD-13C12-
Penta-CDD-13Ci2
Hexa-CDD-l3C12
Hepta-CDD-13C12
Octa-CDD-l3C12
Tetra-CDF-13CI2
Penta-CDF-13Ci>2
Hexa-CDF-13Ci2
Hepta-CDF-13Ci2

32
27
30
30
30
31
31
31
32
%
- Ill
- 130
- 110
- 120
- 130
- 110
- 110
- 110
- 120
Above
26
25
17
13
19
21
23
13
19
Below
2
2
4
5
7
2
2
4
6
Total
23
27
21
23
26
23
25
22
25
The recoveries of internal standards from most samples were above  the QC
criteria rang* indicating better than expected recoveries.  The
recoveries froa the leachate prepared from Sample 17620  (bottom/fly  ash
from Facility A) and from the field leachate sample (19865-63) from
Facility 8, however, were consistently below the QC criteria.  Because
the internal standards are used to correct analytical results  for
extraction efficiency and cleanup losses, however, the failure to  meet
the QC criteria does not affect the quality of the data  provided.
                                   4-74

-------
      Overall.  the  analyses of samples  for PCDDs and PCDFs were in control
 with very low  levels  of  contamination  in blanks, acceptable recoveries of
 analytes from  native  spike samples and generally acceptable to better
 than expected  recoveries of  isotopically labeled internal standards.
 These results  are  consistent with good quality analytical practice.  The
 data is  considered to be acceptable.
      4.5.1.4   Organic Constituents - Analyses of selected field water
 samples  and laboratory-prepared leachates for semi-volatile organic
 compounds  (Base Neutral/Acid Extractable or BNAs) were performed by the
 Versar laboratory.  Analyses of each batch of samples of each matrix were
 accompanied by internal  QC checks consisting of the following analyses:
 analysis of laboratory blanks, determination of recoveries of six
 surrogate  compounds which are readily  identified in the GC/MS analysis
 and  added  to each  sample before extraction to track the performance of
 the  extraction and analysis, and determination of the recoveries of
 matrix spikes  and  matrix spike duplicates {the spikes are added to one
 sample per batch prior to .extraction and analysis) to monitor the
 accuracy and precision of the analysis.  The criteria for recovery of
 surrogates and the matrix spike and matrix spikt duplicates are specified
 in the EPA Contract Laboratory Program and are listed in the summary
 tables in  this section of this report.
     The results of these internal QC  checks for the BNA analyses of
 samples  in this project  are summarized in Table 4.18 and discussed below.
     No  semi-volatile organic compounds were detected in the BNA analyses
 of laboratory blanks for the field water samples indicating that the
 laboratory water and reagents were free of contamination by this group of
 compounds.  Diethyl phthalate was detected in the blanks of the EP, TCLP
 and MWEP leachates prepared in the laboratory at concentrations from  3 to
 24 ug/L.   This is a common occurrence  resulting from leaching of
phthalates from plastic bottles used in preparation of the leachates.
The blanks did not interfere with subsequent analyses.
                                   4-75

-------
                       TABLE 4.18  QC SUMMARY  (INTERNAL) FOR ORGANIC ANALYSIS
                                  Surrogate Recoveries (%) for Field Water Saaples

Hit;
A
A
B
a
a
a
a
a
a
c
c
c
c
c
c
c
c
c
0
0
0
0
0
0
0
0
0
0




Sanple
i Matrix
Quench
Quench
Quench
Quench
Quench
Quench
Leachate
Leachate
Leachate
Leachate
Leachate
Leachate
NWell
dwell
MWell
Quench
Quench
Quench
Leachate
Leachate
Leachate
Leachate
Quench
Quench
Quench
Quench
Quench
Quench
Blank
Blank
Blank
Blank
Sanple
Description
Unit 1. 9/26
Unit 2. 9/26
Unit 3. 9/28
Unit 3, 9/28, 1/10 Oil
Unit 4. 9/28
Unit 4, 9/28, Quo
East Side
North Side
Northeest Corner
North Side
Northeast Comer
Northwest Corner
»17
«
#4
. Unit 2. 9/30
Unit 2. 9/30
Unit 2. 9/30
Northeast Corner
Northeast Corner
Northeast Corner
Southeast Corner
Unit 2. 10/3
Unit 2. 10/3
Unit 2. 10/3. Oup
Unit 2, 10/3. Oup
Unit 2. 10/4
Unit 2. 10/4
Laboratory
Laboratory
Laboratory
Laboratory
Samle
Niober
17538
17548
17588
17588
17598
17528
19833
19861
19848
19811
19795
19823
19781
19755
19768
19558
19558 MS
19558 MSO
19628
19615
19618RE
19602
19641
1W43RE
196S3
19656RE
19694
19697RE
RB587
R8S87
RB599
RB686
Nitro
Senzene-05
99
87
103
78
97
93
91
90
92
72
103
91
87
101
95
100
99
105
81
28"
55
67
76
64
88
63
68
72
74
88
72
9«
2-Fluoro-
Blphenyl
87
74
96
84
85
94
79
52
72
66
62
81
77
90
86
96
96
103
65
61
59
33
30-
25»
29-
27-
31-
25-
84
90
76
94
Terphenyl
-04
109
as
108
97
90
95
86
46
57
58
38
118
119
131
129
112
111
112
36
8»
23*
22-
14-
26»
19-
30«
9-
0-
101
112
115
108
Phenol
-05
84
36
96"
37
94
96"
35
93
90
68
91
79
32
77
70
77
77
82
37
47
56
69
39
71
104*
83
104*
73
43
72
72
90
2-F1uor
Pneno
94
36
95
95
38
92
75
31
87
73
75
75
34
30
71
92
32
36
28
33
38
63
79
74
91
77
100
69
61
70
76
99
               QC Limits
36-114     43-116    33-141     10-94     21-100
                                                                                             Phenol

                                                                                              114
                                                                                               36

                                                                                              113
                                                                                               30
                                                                                               73
                                                                                               34
                                                                                               94
                                                                                               91
                                                                                               34

                                                                                               48
                                                                                               38
                                                                                               83
                                                                                               44
                                                                                               35
                                                                                               72
                                                                                              100
                                                                                               93
                                                                                               97

                                                                                               93
                                                                                              103
                                                                                              103
                                                                                               99
                                                                                               34
                                                                                               18
                                                                                               45
                                                                                               20
                                                                                               35
  61
  59
  69
  79

10-123
LEGEND:
         MS • iwtrlx spike saiple
         HSO • ntrlx spike duplicate saeple
         RE • saiple was rtextracted and analyzed
         • - value exceeds the QC Halt
                                       4-76

-------
                       TABLE 4.18  QC SUMMARY (INTERNAL)  FOR  ORGANIC ANALYSIS
            Surrogate Recoveries (%) for Laboratory Leachates  (EP.  TCLP. and SW-924)

Samp It
Facility Matrix
A
A
A
A
3
a
c
c
0
0


A
A
B
C
0
0


c
0
0
0
0

tot torn/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Fly
Bottom
Bottom/Fly
Fly
Fly
Bottom/Fly
Blank
Blank
Bottom/Fly
Bottom/Fly
Botton
Fly
Fly
Bottom/Fly
Blank
Blank
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
BottOM/Fly
Blank
Leaching
Procedure
EP Toxldty
EP Toxlclty
EP Toxldty
EP Toxlclty
EP Toxldty
EP Toxldty
EP Toxlclty
EP Toxldty
EP Toxldty
EP Toxlclty
HA
NA
TCLP
TCLP
fCLP
Tap
TCLP
Tap
NA
NA
SW-924
SW-924
SW-924
SM-924
SH.924
NA
Staple
Nltro
Nuefcer Benzene-OS
17651
17651MS
17651MSD
176510up
17695
17694
19517
19521
19673
19678
RB701
BUnk
17651
176510up
17694
19521
19673
19678
RB701
Blank
19517
19678*1
19678*2
19678NS
19678MSO
RB712
104
109
107
105
103
104
121*
92
94
98
102
63
111
90
122«
103
107
109
102
108
78
101
93
105
114
89
2-Fluoro-
Blphenyl
94
98
90
95
89
91
108
96
90
94
109
68
87
90
100
84
36
36
109
97
96
82
31
89
92
78
Terphenyl
-04
96
103
98
99
52
57
108
97
70
95
120
60
36
84
84
79
73
32
120
34
66
43
75
83
86
87
Phenol 2-Fluoro- 2
-OS
7«
55
78
76
67
13
10
29
39
51
90
74
34
81
42
12
92
66
90
106*

91
90
85
36
38
Phinol
33
31
34
34
86
3«
57
4«
6'
7*
81
33
18-
SO
5«
2"
61
10«
31
91

83
31
30
31
38
,4,6-Tribronn
Phenol
12
20
71
70
67
5-
15
6«
7«
9«
69
73
21
66
8«
6«
74
18 .
69
67

91
38
91
36
39
               QC Lialts
36-114
43-116    33-141    10-94    21-100
10-123
LEGEND:
         MS • Mtrlx spike
         HSO • Mitrlx splk* duplicate saeple
         RE • saeple MU reextracted and reanalyzed
         • • value exceeds the QC Unit
                                          4-77

-------
                        TABLE 4.18  QC  SUMMARY  (INTERNAL) FOR ORGANIC ANALYSIS
                          Matrix Spike  Results  for Field Water Samples (Precision and Accuracy)

SPIKE COMPOUND
Base/Neutral Extractives
1 , 2 . 4-Tr ich lorooenzene
Acenapntnene
2.4-Ofnitro Toluene
Pyrene
N-N 1 troso-0 1 -n-Propy laml ne
1,4-Oichlorobenzene
Acid Extractables
Pentachloropnenol
Phenol
2-Chlorophenol
4-Ch loro- 3-Methy 1 pheno 1
4-Nitropnenol
Facility C
, Quench
Water
Saiple No. 19558
MS
88
86
77
34
88
83

31
77
79
36
23
MSO
91
92
30
38
95
36

33
3*
33
90
18
Matrix Spike


SPIKE COMPOUND
Base/Neutral Extractables
1 . 2. 4-Trich lorooenzene
Acenaphtnene
2,4-OinUro Toluene
Pyrene
N-Nltroso-Oi-n-Propylamine
1 . 4-0 1 ch 1 orobenzene
Acid Extractables
Pentactilorophenol
Phenol
2-Chlorophenol
4-Ch 1 oro-3-nethy I pheno 1
4-Nltroptwnol
EP Toxldty
Facility A.
Sanple No
MS
32
84
90
89
88
80

24
51
43
• 38
as
RPO
3
7
4
5
3
4

2
9
5
5
24
Results
Leachate
Sot ton/Fly
. 17651
MSO
83
83
91
88
89
31

71
72
71
88
98

RPO
1
1
1
1
1
1

101*
34
50"
1
IS
Facility C. Well Water
Saaple No. 19768
MS
90
87
119«
120
84
82

58
72
72
85
78
for Laboratory
SW-924
Facility
Samplt No
MS
77
78
69
76
84
75

36
93
84
34
39
MSO
36
82
107"
116
77
76

57
67
67
76
69
Leachates
Leacnate
RPO
5
6
19
3
7
8

2
7
7
11
10
(Precision

qc
RPO
28
31
38
31
38
23

50
42
40
42
50
Limits (*)
Recovery
39-98
46-113
24-96
26-127
41-116
36-97

9-103
12-39
27-123
23-97
10-80
and Accuracy)


0. 3otton/F1y
. 19678 Dup
MSO
79
79
73
76
90
75

82
91
34
85
78
QC Limits (%)
RPO
3
1
6
0
7
0

5
2
0
1
13
RPO
28
31
38
31
38
28

50
42
40
42
50
Recovery
39-98
46-118
24-96
26-127
41-116
36-97

9-103
12 -8S
27-123
23-97
10-30
LEGEND:
MS • matrix spike saaple
MSO • matrix spike duplicate saeple
RPO • relative percent difference'
• • value exceeds the QC Halt
                          4-78

-------
      The criteria for recovery of surrogate  compounds  were generally
 achieved in the analyses of field water samples  and laboratory-prepared
 leachates, with some exceptions.   The Versar laboratory  encountered
 difficulties with low recovery of the two heavier  base neutral
 extractable compounds (2-fluoro biphenyl and terphenyl-04) in analyses of
 leachates and quench water from Facility 0.   Four  samples were
 re-extracted and reanalyzed with  similar or  poorer results indicating
 matrix interferences in the extraction and analysis.   Problems with low
 recoveries were encountered also  with the two heavier  acid extractable
 surrogates (2-fluorophenol and 2,4,6-tribromophenol) in  analyses of the
 EP and TCLP leachates.   Mo acid extractable  compounds  were detected in
 the analyses of samples,  however,  so  this problem  is of  no consequence.
      The  criteria  for recoveries  of Matrix Spike (MS)  and Matrix Spike
 Duplicates (MSD),  and for the  Relative Percent Difference (RPD) between
 the two were generally achieved.   No  recoveries  below  the criteria were
 encountered.   The  precision (RPD)  criteria of two  of the acid extractable
 spikes  (pentachlorophenol and  2-chlorophenol) in the analysis of the EP
 leachate  of  bottom/fly ash from Facility A were  exceeded.
     Overall,  the  analyses for BNAs in the field water samples and
 laboratory-prepared  leachates  were in control.   The data from the
 analyses  of  samples  are,  therefore, considered valid.  Corrective actions
 were taken by  the  laboratory on each  occasion of a criteria exceedance in
 accordance with the  Contract Laboratory Program  protocol.
     The  total organic  carbon  (IOC) analyses  and organic scans w«re also
 accompanied by internal quality control  checks.  These included analyses
 of  reagent and calibration blanks, analyses of check standards, and
 analysis of an EPA quality control sample (WP-1248 for TOO and WP-379 for
 organic scan).  The  blanks  were below the detection limits of the
methods.  Recoveries  in analyses of the  check standards  and the EPA QC
Standards ranged from 92  to 110 percent,  within  the QC criteria of 90 to
 110 percent specified in  the Quality  Assurance Project Plan.
                                   4-79

-------
      4.5.2   External  QA/QC
      The  external QA/QC  samples were field duplicate samples collected at
 a frequency  of  25 percent.  These samples were submitted to the laboratory
 as "blind" QC samples (i.e., the analysts were not aware that these
 samples were duplicates) to evaluate the precision of the entire sampling
 and analysis method.   The analytical results of these external QA/QC
 samples are  presented and evaluated in the following sections.
      4.5.2.1 Metals  - The results of the field duplicate analyses for
 metals and the  relative percent differences (RPD) for these duplicate
 analyses are presented in Table 4.19.  These results are summarized by
 sample matrix and facility.
      A review of the  bottom/fly or bottom ash field duplicate samples
 revealed the following.  The precision for selenium and cadmium was the
 best, while  iron, manganese, and zinc had the worst precision.  The
 precision for Facility A was the best, followed by Facilities 3, C,
 and D, sequentially.   Finally, although the field duplicates had the
 increased variability  of sampling, 17 of 44 sample parameter results had
 RPDs of <20  percent, which is the RPD criteria for duplicate metals
 analyses.
     A review of the fly ash field duplicate samples showed the following.
 First, the precision for the manganese duplicate analyses was the best,
 and the precision for  the cadmium duplicate analyses was the worst.  The
 precision for Facility B was the best, followed.by Facilities A, C,
and 0, sequentially.  Finally, the RPD was <20 percent for 41 of 44
analyses.   It was expected that the precision of the fly ash field
duplicates would be better than the precision of the bottom/fly or bottom
ash field duplicates because of the more homogeneous nature of the fly
ash samples.
     A review of the quench water field duplicate samples showed the
following.  First,  the RPDs at Facility B were much better than those at
Facility D.   This was  expected because of the quantity of floating solids
                                   4-30

-------
                                TABLE 4.19  QC  SUMMARY (EXTERNAL) FOR HETALS
                                       TOTAL METALS IN SOLID SAMPLES
'lant
A
A

C
C

0
0

A .
A

3
3

C
C

0
0

B
8
Sample
: M«tr1x
Bottom/Fly
Bottom/Fly
RPO (%)
Bottom/Fly
Bottom/Fly
RPO (%)
Bottom/Fly
Bottom/Fly
RPO (%)
Fly
Fly
RPO (%)
Fly
Fly
RPO (%)
Fly
Fly
RPO (%)
Fly
Fly
RPO (%)
Botto*
Bottoa
Cd
ng/kg
17
15
12.5%
24
27
11.3%
17
18
5.7%
193
186
3.7%
322
316
1.9%
191
157
19.5%
259
172
40.4%
3.8
3.5
Cr
ng/kg
12
16
28.6%
19
26
31.1%
31
36
14.9%
79
66
17.9%
105
98
6.9%
54
52
3.8%
77
67
13.9%
66
78
Cu
ng/kg
369
377
2.1%
3420
608
139.6%
289
728
36.3%
2380
2040
15.4%
745
724
2.9%
531
556
4.6%
516
518
0.4%
792
581
Fe
ng/kg
6650
9140
31.5%
5040
9720
63.4%
8590
95100
166.9%
17400
15000
14.8%
9900
9350
5.7%
8200
8450
3.0%
8320
7190
14.6%
115000
24100
Pb
ng/kg
2200
1140
63.5%
1700
1060
46.4%
571
612
6.9%
5550
5400
• 2.7%
7350
7270
1.1%
3490
3130
10.9%
5450
4600
16.9%
2140
3930
Mn
184
251
30.8%
155
1810
168.4%
3130
640
132.1%
1010
1020
1.0%
895
389
0.7%
388
382
1.6%
857
751
13.2%
1010
938
H1
22
24
8.7%
42
38
10.0%
26
119
128.3%
106
91
. 15.2%
30
76
5.1%
102
95
7.1%
63
55
13.6%
36
90
Zn
ng/kg
1730
3050
55.2%
1570
3250
69.7%
2400
46000
180.2%
15700
14500
7.9%
32700
31800
2.8%
10300
8460
19.6%
22100
18600
17.2%
2350
5760
AS
ng/kg
7.9
12.2
42.3%
5.7
7
20.5%
5.4
6.1
12.2%
41.9
38.0
9.3%
106
89.9
16.4%
16.2
17.7
3.8%
50.7
54.5
7.2%
3.9
6.9
S«
rag/kg
<5
0.0%
<0.5
163.6%
:;
0.0%
<5
«5
0.0%
«!S
0.0%
7.6
5.2
20.3%
9.6
9.1
5.3%
;;•
Hg
nq/kg
6.9
5.0
31.9*
0.62
0.13
110.0*
0.21
0.13
47.1*
27.
23
16.0*
9.3
3.0
15. M
5
4.0
22.2*
1.8
2.0
10.5*
0.12
0.12
RPO (%)
8.2%    16.7%    30.7%   130.7%    59.0%     7.4%    85.7%    84:1%    25.3%
0.0%
0.0*
                                                4-81

-------
                              TABU 4.19  QC  SUWMftY (EXTERNAL)  FOR HETALS
                                     TOTAL METALS IN LIQUID SAMPLES
Sample
Plant Matrix
a
8

0
0

Quench
Quench
RPQ (%)
Quench
Quench
RPO (%)
Cd
ug/L
<5.0

-------
                   TABLE 4.19  QC SUMMARY (EXTERNAL) FOR METALS
         Matrix
Plant  (Leaciutc)
  Fly
 (TCLP)

RPO (*)
  0       Fly
  0   (SW924-CX1)

        RPO  (%)

  0       Fly
  0   (SH924-EX2)

        RPO  (%)
  Cd
 «Q/L
        Cr
       «g/L
                                Cu
                               mg/L
                  Ft
                 mg/L
   10.3
   8.90
0.487    0.018
0.544   0.0059
                           12.8
                           15.0
  0.015    0.071   0.0052   <0.005
  <0.01    0.114   0.0051   <0.005
              100.0%    46.5%
                      1.9%
                            0.0%
  <0.01    0.116   
-------
 in the quench water from Facility D.  Second, the RPDs for selenium and
 mercury analyses were the best, while the RPDs for copper, iron, and zinc
 were the worst.  Finally, the RPD was <20 percent for 13 of 22 analyses.
     A review of the laboratory leachate field duplicate samples revealed
 the following.  First, the precision of the EF method was good for
 cadmium, chromium, manganese, arsenic, selenium, and mercury and was poor
 for copper, iron, and lead.  The RPD was <20 percent for 13 of the 22 EP
 leachate duplicate parameters.  Second, the precision for the EP method
 was ouch better than for the TCLP and MWEP (SW924) methods.  The RPD was
 <20 percent for 11 of 22 TCLP duplicate parameters.  Finally, for the
 MWEP method, only two out of 21 sample parameters which were detected had
 an RPO of <20 percent.
     Overall, the quality control results for metals based on the
 differences between duplicate samples did not suggest the presence of a
 significant systematic error.  Some random errors are inevitable in a
measurement (sampling and analysis) process.  The random anomalies, that
did occur with the metals data were isolated and did not affect
 subsequent interpretations of the data.
     4.5.2.2  PCBs - The results of the duplicate analyses of selected
 samples for individual PCS homologs and total PCBs are summarized by
 sample matrix and facility and presented in Table 4.20.
     A review of the results for fly ash field duplicate samples revealed
 the following.  The RPO increased as the level of chlorination
 increased.  The RPD ranged from 0.0 percent to 4S.5 percent  for total
PCBs and from 0.0 percent to 81.0 percent for individual PCS homologs.
     A review of the results for the analysis of combined  ash and bottom
ash field duplicate samples provided minimal  information because  no PCBs
were detected in field duplicate samples from Facilities A,  B,  and  C.
However, the RPDs for the combined ash from Facility  0  ranged  from
 100 percent to 134.7 percent for the individual  PCB homologs,  and the  RPD
                                    4-84

-------
               TABLE 4.20  QC SUMMARY (EXTERNAL) FOR PCB ANALYSIS
                    QC RESULTS FOR SOLIDS
Plant
A
A

A
A

3
8

a
3

C
C

C
C

0
0

0
0
HOMO
Sup It -C8
H«tH« (ng/g)
F1y Ash
Fly Ash
RPO (%)
8otto«/Fly
BottM/Fly
RPO (%)
Fly Ash
Fly Ash
RPO (%)
BottM
Bottom
RPO (%)
Fly Ash
Fly Ash
RPO (%)
Bottoa/Fly
BottostfFly
WO (*)
Fly At*
Fly Ask
W0(»)
Bottc^Fly
BottosVFly
01 TR1 TETRA PENTA TOTAL
-CB -CB -CB -C8 PCB
(ng/g) (ng/g) (ng/g) (ng/g) (ng/g)
0.70 0.70
0.73 0.73
4.2% 4.2%
NO
NO
0.0%
NO
NO
0.0*
NO
NO
0.0*
«0.20 «0.20
0.81 0.81
154.0* 158.0*
NO
NO
0.0*
2.88 2.91 2.41 8.20
2.42 1.72 1.02 5.18
17.4* 51.4* 31.0* 45.5*
<0.20 2.79 -0.20 2.79
1.3S 14.3 18.5 32.15
RPO (*)
172.4*   134.7*   197.8*
168.1*
                          4-35

-------
                      TABLE  4.20   QC SUMMARY (EXTERNAL) FOR PCS ANALYSIS
                           QC RESULTS FOR LIQUIDS
                    MONO
         SaipU      -CB
Plant Description   ug/L

  0   Field Leachate
  0   Field Leachate
01
-ca
ug/L
TRI
-CB
ug/L
TETRA
.CB
ug/L
PENTA
-CB
ug/L
TOTAL
PCS
ug/L
                                            NO
                                            NO
        RPO (%)

  3   Quench Hater   0.002
  3   Quencti Meter    0.03
        RPO (%)

  0   Quench Meter
  0   Quench Mater

        RPO (%)
175.0*
  0.0%

0.002
 0.03

175.0%

NO
NO

  0.0%
        LEGEND:
                  HOW -C3 - Monochlorlnated Blphenyl
                  01 -C3 - 01chlorinated Blphenyl
                  TRI .C8 • THchlorlnated Blpnenyl
                  TETRA -C8 - Tetrichlorlnated aipheny)
                  PENTA -CB - PentaehloHnated 31ph«ny1
                  NO • Not Detected
                                 4-86

-------
 for the total PCBs was 168.1 percent.  This large RPD nay be attributed
 to the heterogeneous nature of the combined ash samples.
      A review of results from the analysis field water duplicate samples
 showed that for a majority of the duplicates no conclusions of the
 precision could be made because of the extremely low concentrations of
 PCBs.
      4.5.2.3  PCDD/PCDFs - The results of the duplicate analyses for
 individual and total PCDD and PCDF homologs is presented  in Table 4.21.
 These  results are summarized by sample matrix and facility.
     A review of the fly ash data for PCDD/PCDF field duplicate sample
 analyses  revealed the following.   First,  19 of 24 PCDD and 14 of 20 PCDF
 duplicates had an RPD of <20 percent.  Second, the precision of the PCDDs
 was  slightly better than that of  the PCDFs.  Third, the RFDs increased as
 the  concentrations  of the individual homologs increased.   Fourth,  the
 PCDD precision was  best for Facilities C  and D,  while the PCDF precision
 was  best  for Facilities A and B.   Finally,  the precision  for the
 tetra-chlorinated classes of both PCDD and PCDF were best,  while the
 precision  of the  hepta-chlorinated classes  of both PCDD and PCDF were
 worst.
     The  results  from the combined ash and bottom ash field duplicate
 sample analyses showed the  following.   First,  5  of 12 PCDD  and 1 of
 12 PCDF duplicate results had an  RPD of less than 20 percent.   This
 decreased  precision among the combined/bottom ash duplicates is a result
 of the heterogeneity  of the samples.   Second,  the precision for the PCDDs
 was slightly better than  for the  PCDFs.   Third,  the RPOs  decreased as the
 concentrations of the  individual  homologs increased.   Fourth,  both the
 PCDD and PCDF precision was better for Facility C than for  Facility B.
 This may be  a result of the Facility C duplicate samples  being combined
 bottom/fly ash, while  the Facility B duplicate samples were  exclusively
 the more heterogeneous  bottom ash.   Finally,  the precision  was best for
 the octa-CDD and octa-CDF homologs  and was  worst for the  penta-CDD and
hepta-CDF homologs.
                                   4-87

-------
            TABLE 4.21  QC SUMMARY (EXTERNAL) FOR PCDO/PCDf ANALYSIS
                 QC RESULTS FOR SOLIDS (OIOXIN HOMOLOGS)


Plant
A
A

3
3

B
a

c
c

c
c

0
0

Saaplt
Matrix
Fly Ash
Fly Ash
RPO
Fly Ash
Fly Ash
RPO
Bottom Ash
Bottom Ash
RPO
Fly Ash
Fly Ash
RPO
Bottom/Fly
Bottom/Fly
RPO
Fly Ash
Fly Ash
2,3,7,8
TCDO
"9/9
0.093
0.11
16.7%
0.38
0.38
0.0%
<0.08
0.01
120.0%
1.5
2.1
33.3%
0.62
0.78
22.9%
0.38
0.45
TETRA
.coo
"9/9
2.3
2.8
19.6%
12
11
8.7%
<0.08
0.11
93.3%
31
33
6.3%
14
13
7.4%
5.2
5.1
PENTA
-COO
"9/9
11
14
24.0%
139
114
19.8%
<0.05
0.21
157.4%
710
722
1.7%
47
SO
6.2%
54
46
HEXA
•COO
"9/9
20
20
0.0%
126
123
2.4%
0.07
0.16
78.3%
5565
3946
34.0%
67
78
15.2%
105
103
HEPTA
-COO
"9/9
14
14
0.0%
100
93
7.3%
0.13
0.24
59.5%
1759
3030
53.1%
120
120
0.0%
49
48
OCTA
-COO
"9/9
17
18
5.7%
96
39
7.6%
0.35
0.61
54.2%
2460
3152
24.7%
89
39
0.0%
44
48
TOTAL
-COO
"9/9
64.3
68.3
6.8%
473
430
9.5%
0.55
1.33
83.0%
10525
10883
3.3%
337
350
3.8%
253.2
250.1
•RPO
16.9%    1.9%   16.0%    1.9%   6.5%    8.7%    1.2%
                             4-88

-------
           TABLE 4.21  QC SUMMARY (EXTERNAL)  FOR PCDO/PCDF ANALYSIS
                 QC RESULTS FOR SOLIDS (FURAN  HOHOLOGS)


Fac.
A
A

a
a

a
a

c
c

c
c

0
0

Sup It
Matrix
Fly Ash
Fly Ash
RPO
Fly Ash
Fly Ash
RPO
Bottoa Ash
aottM Ash
RPO
Fly Ash
Fly Ash
RPO
Bottom/Fly
Bottom/Fly
RPO
Fly Ash
Fly Ash
2.3,7.3 TETRA
TCOF -OJf
ng/g ng/g
20
23
14.0%
91
97
6.4*
0.05 0.28
0.09 0.68
57.1* 83.3%
164
169
3.0%
2.9 20
3.8 24
26.9% 18.2%
36
36
PENTA
-CDF
ng/g
7.1
10
33.9%
64
65
1.6%
0.18
0.33
58.8%
221
22S
2.2%
20
27
29.8%
32
27
HEXA HEPTA
-COF
ng/g
17
14
19.4%
56
61
3.5%
0.1
0.26
88.9%
336
2353
150.0%
24
35
37.3%
115
21
-OJf
ng/g
14
12
15.4%
40
40
0.0%
0.1
0.26
38.9%
32
77
82.6%
27
36
28.6%
80
3.8
OCTA TOTAL
-CDF
ng/g
2.1
2.3
9.1%
3.1
8.3
2.4%
0.06
0.12
66.7%
60
362
143.1%
6.7
8.4
22.5%
4.9
5.6
-COF'
ng/g
60.2
61.3
1.3%
259.1
271.3
4.6%
0.72
1.65
78.5%
313
3187
118.7%
97.7
130.4
28.7%
267.9
93.4
PCOO *
PCOF
ng/g
124. S
130.1
4.4%
732.1
701.3
4.3%
1.27
2.98
30.5%
11338
14070
21.5%
434.7
480.4
10.0%
521.1
343.5
RPO
0.0%   16.9%  138.2%  181.9%   13.3%   96.6%    41.1%
                             4-89

-------
                     TABLE 4.21  QC SUJftARY  (EXTERNAL) FOR PCOO/PCOF ANALYSIS


                           QC RESULTS FOR  LIQUIDS  (OIOXIN HOHOLOGS)
                   2.3.7.8  TETRA   PENTA     HEXA   HEPTA    OCTA   TOTAL
         Sup It      TOO"    -COO    -COO     -COO    -COO    -COO    -COO
Plant    Matrix     (ng/1)  (ng/1)   (ng/1)   (ng/1)  (ng/1)  (nq/1)  (ng/1)

  0  Field leachate  <0.22    0.13      0.4     2.2     8.2      23   33.93
  0  Field Leachate  <0.26    0.27    <0.22     2.1     3.3      25   36.17

          RPO         16.7%   70.0%  113.7%   4.7%    7.1%    3.3%    6.4%

  3   Quench Water   <0.07   <0.07    <0.03    <0.01   <0.03    0.06    0.06
  9   Quench Hater   <0.07   <0.07    
-------
      The results  for the field leachate  and quench water field duplicate
 samples analyses  showed the following.   First.  9  of 13  PCDO and 10  of
 13 PCDF duplicate results had an RPD of  less than 20 percent.   Second,
 the precision was better for the PCDFs than for the PCODs.   Third,  the
 precision was also better for the field  leachates than  for  the quench
 water samples, which was expected because the quench water  samples
 contained floating solids that added to  their heterogeneity.   However,
 these results are misleading because the PCOD and PCDF  concentrations
 were  near the detection limits,  which make  the  RPDs unrepresentatively
 high.   Finally, the  precision was best for  the  octa-CDD and tetra-CDF
 homologs,  and was  worst for the  tetra-CDD and penta-CDF homologs.
      Overall,  the  quality of the PCDD/PCDF  data appeared to be excellent
 therefore  suggesting that the  data could be  used  with a high degree of
 confidence.
      4.5.2.4  Organic Constituents - The results  of the duplicate
 analyses for organic constituents  are presented in Table 4.22.   This
 table shows that the precision is  generally  good.   Relative percent
 differences were not calculated  because  of the nature of the analysis and
 the multitude of BNA compounds which were tentatively identified.
Therefore, any calculation of  RPDs would not be representative of the
actual sampling and analysis precision,  due  to the  nature of the
analytical method.
                                   4-91

-------
                                  TABLE 4.22  QC SUMMARY (EXTERNAL) FOR ORGANICS
         Sample
Plant Description
      Held Leacha
      Fit Id leacha
Ethyl Dimethyl


TOC



(ng/1)
636
567
.0
.0

Organic
Scan
Ong/1)
<0.25

BNA
Peaks
Found
(No.)
22
24
Hexyl
Phthalate
117817
(ug/L)
80
37
Propane
Olol
126307
(ug/L)
110
120

Blphenyl
90437
(ug/L)
51
51
MM
TTHepant
17233715
(ug/L)
82


Thlolane
289167
(ug/D
400
140



Unknown
HCs
(#)




9
10
Unknowns
(#)
8
10
Plant
   Saople
   Matrix
                                                                             2-Hydroxy
                  BNA            2-Methyl  4-Hethyl  Benzole Molecular          Benzole
        Organic   Peaks   Phenol   phenol   phenol    Acid    Sulfur  Thlolane   Acid
 TQC     Scan    Found    108952    95487    106445    65850 10544500  289167    69727
(•B/l)   (ms/1)    (Ho.)   (ug/L)   (ug/L)   (ug/L)   (ug/L)   (ug/L)   (ug/L)   (ug/L)
  B   Quench Water  421.0     «0.25       20      380       40      92     2100       29
  3   Quench Mater  416.5     <0.25       20      380       44.      94     2100      130
                                                                                       23
                                                                                   SO
                                                                                   42
Plant
            Hexanoic
              Add
   Sample    142621  Unknowns
   Matrix    (ug/L)     (»)
  8   Quench Water     58       13
  a   Quench Water     37       12
Plant

  0
  0
   Sanple
   Matrix
                                                                              Methyl
                   BNA           2-Hethyl 4-Methyl  Benzole   Hexyl  Hexanoic Pentanolc
        Organic   Peaks   Phenol   phenol   phenol    Acid   Phthalate  Add     Add
 TOC     Scan     Found    108952    95487   106445    65850   117817   142621   646071
(mg/1)  (av/1)    (No.)   (ug/L)   (ug/L)   (ug/L)   (ug/L)    (ug/L)    (ug/L)   (ug/L)
Quench Water  165.0
Quench Water  153.0
          «0.25
25
25
60
71
23
570
900
45
51
17
34
         Samle
                     Methyl     Furan   Benzene   Tetra   Methyl
             Benz-  Pentane-  Carbox-  Propanotc Oeeanoic Purlne
            aldehyde  dlol   aldehyde   Acid     Add     done   Unknown  Unktmn
             100527   144194    67470   501520   544638    58082 Org Acids   HCs   Unknowns
Plant    Matrix    (ug/L)  (ug/L)    (ug/L)    (ug/L)   (ug/L)   (ug/L)
                                                                   (#)
                                                                        (*)
  0   Quench Water
  0   Quench Water
                 22
             17
         23
         12
        4-92
                  23
                  22
                            9
                           17

-------
  5.0   EVALUATION
       In this  section, the data presented and discussed in Section 4.0 are
  summarized and evaluated.  To facilitate this evaluation, the data were
  averaged by facility, sample type, and analytical parameter
  combinations.  Then, the data were evaluated with respect to previously
  reported information, variations between sample types, variations between
  laboratory leachate preparation procedures, municipal waste combustor
  (MWC) facility design and operation, and characterization of the residues
  as hazardous wastes.  Section 5.1 presents the concentration ranges for
  each sample type and analytical parameter from this study and compares
  them to  the concentration ranges from previous studies.   Section 5.2
  presents the data summary tables and an evaluation of the significant
  trends observed from these tables.  Section 5.3 provides a qualitative
 evaluation of the relationships between MWC facility design and operating
 characteristics  and the  concentrations of constituents in the residues.
 Finally, Section 5.4 presents an overall assessment of the hazardous
 waste characteristics of the  MWC residues based on existing standards and
 criteria.
   .   5.1 Comparative Evaluation With Previously Reported Information
      The data  extracted  from  the  documents  identified in the literature
 review (see Section 2.0)  were summarized by sample type  and analytical
 parameter.  From  the  summarized  data,  a  concentration range was
 determined for each sample type/analytical  parameter combination from the
 previous studies.   The lower  end  of  any  given  range  was  the miriimum
 concentration  reported in any previous study for that particular sample
 type/analytical parameter combination.   Similarly,  the upper end of any
 given  rang* was the maximum concentration reported in any previous  study
 for that  particular sample type/analytical  parameter combination.   Using
 an analagous approach, the concentration range was determined for each
 sample type/analytical parameter  combination from this study.   However,
previous  studies did not provide  any data for PCDD/PCDFs  or organic
constituents (i.e., BNAs) in  laboratory-prepared leachates,-or
                                    5-1

-------
 for PCBs or PCDD/PCDFs in field water samples (i.e., quench water, field
 leachate, and ground water).  Sections 5.1.1 through 5.1.3 present the
 concentration ranges from this study and from previous studies for the
 available sample type/analytical parameter combinations and provide a
 narrative evaluation of the findings.
     5.1.1  Solid Samples
     The concentration ranges for metals in fly ash and combined ash are
 presented in Table 5.1.  As can be seen from this table, the results for
 the fly ash from this study are within the concentration ranges from
 previous studies for all metals except copper, mercury, and selenium,
 where Versar's results are slightly higher.  Similarly, for the combined
 ash,-the results from this study are within the concentration ranges from
 previous studies for all metals except copper and zinc.  One possible
 explanation for these discrepancies may be that in several of the previous
 studies, only one MWC facility was sampled, and the concentration range
 arising from the sampling, analytical/ and operational variability at one
 facility would not be expected to encompass the concentration range
 resulting from four different facilities.  Generally, the results for
 both the fly ash and combined ash from this study extend fcom the low and
 to the midpoint of the range from the previous studies.
     The concentration ranges for PCBs in fly ash and combined ash are
 presented in Table 5.2.  Both the fly ash and combined ash results from
 this study are within the concentration ranges from previous studies for
 every individual PCS homolog, as well as for total PCBs.  Generally, the
 results from this study are near the lower end of the ranges from the
previous studies for both ash types.  One noteworthy trend is that the
higher chlorinated species of PCBs (i.e.. the hepta- through deca-
 chlorinated species) were not detected either in this study or in the
previous studies, except for negligible concentrations of hepta-CB and
octa-CB in the fly ash.
                                    5-2

-------
                     TA8U 5.1  COMPARATIVE EVALUATION OF TOTAL METALS IN SOLID SAMPLES
                                                  FLY ASH
 fetal
 Arsenic  (As)
 Caoftlua  (Cd)
 Chronlua (Cr)
 Copptr (Cu)
 Iron  (Fe)
 Lead  (Pb)
 Manganese  (Mn)
 Mercury  (-Kg)
 Nickel (HI)
 Seleniun (Se)
 Zinc  (In)
Concentration Rang* Fro*
   This Study (ng/kg)

        16 • 149
       107 - 475
        48 - 105
       484 . 2.380
     5,960 • 22.300
     2,830 - 14,400
       320 - 1,410
      0.94 - 35.0
        52 • 245
     N0(5) - 15.6
     8,460 - 38,800
Concentration Rang* Fro*
Previous Studies (ng/kg).
              References
       4.3 - 750
       5.0 - 2,210
        21 - 1,900
       187 • 2.300
       900 - 37,000
       200 - 26,600 •
       171 - 3.500
  N0(0.02) - 6.77
   N0(1.5) . 3.600
   N0(0.2) - 12
     2.800 - 152.000
                  42, 53
                  34, 42
                  34, 53
                    53
                  34, 53
                30. 42. 53
                  34, 53
                  30, 53
                    46
                    30
                30, 42. 53
                                             COMBINED ASH [2]
Metal
Arsenic (As)
Cadniua (Cd)
Chroalue) (Cr)
Cdpper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Nickel (N1)
Selentue (Se)
Zinc (In)
Concentration Range Fro*
   This Study (ng/kg)

       2.2 - 24.6
       1.1 - 45.0
        12 - 332
       193 - 10,700
     2.100 - 115.000
       259 • 13,200
       110 - 3.130
      0.11 • 8.7
        13 - 556
   NO(O.S) • 1.4
       54S - 46,000
Concentration Rang* Fro*
Previous Studies (mg/kg)
              References [1]
       0.8
      0.18
        13
        40
       690
        31
        14
  N0(0.02)
   W(l.S)
   W(0.2)
        92
50
100
1.500
3,400
133.500
36.600
4.800
17.5
12.910
50
7,000
    53
    53
30, 42. 53
    53
    53
    53
  46, 53
  30, 53
  46, S3
    53
  46, 53
W  - Not detected: tht detection Halt is given  in parentheses following NO.
[1] • The niaBer(s) in the reference coluen corresponds to the reference iteai nuefcer  in Appendix A  from
      which the conctntratlon range froB previous studies was extracted.
[2] - The concentration ranges were derived froai both combined bottoaVfly and discrete bottoe) ash sanples.
                                                 5-3

-------
                        TABLE 5.2  COMPARATIVE EVALUATION OF PCBs IN SOLID SAMPLES
                                                 FLY ASH
PCS How log
Mono-CB
01 -CB
Tr1-CB
Tetra-CB
Penta-C8
Hexa-CB
Htpta-CB
Octa-CB
Nona-CB
Dtca-C8

TOTAL PCBs
PCS Homo log
Conctntratlon Rang* Fnm
This Study (ng/g)
NO(O.l) • 1.46
NO(O.l) - 7.37
NO(O.l) - 7.67
NO(O.l) - 5.52
NO(O.l) - 2.25
NO(O.l)
NO(O.l)
NO(O.l)
NO(O.l)
NO(O.l)
NO(O.l) - 24.8
COMBINED ASH [2]
Conctntratlon ftangt From
This Study (ng/g)
NO(O.l)
NO(O.l) - 1.35
NO(O.l) - 14.3
NO(O.l) • 16.5
NO(O.l)
NO(O.l)
Itt(O.l)
NO(O.l)
NO(O.l)
NO(O.l)
NO(O.l) - 32.2
i 1 1a1t Is givtn tn partnthtw
Conctntration ftangt Fro»
Previous Studies (ng/g)
NO(O.Ol) - 9.7
NO(O.l) - 10
NO(O.l) - 25
0.5 - 470
NQ(O.l) - 130
NO(O.l) - 55
NO(O.Ol) • 0.2
NO(O.Ol) • 2.5
NO(O.Ol)
NO(O.Ol)
NO(O.l) - 250

Conctntration Rangt Fro*
Prtvlous Stud Its (ng/g)
NO(O.Ol) - 1.4
NO(O.l) - 5.5
NO(O.l) • 30
NO(O.l) . 47
HO(O.l) - 48
NO(O.l) - 39
NO(O.Ol)
NO(O.Ol)
NO(O.l)
NO(O.l)
NO(O.l) - 180
is following NO.
k i tmfmvmnrm i +•• n i^Mf» i n

References [I]
35. 76
35, 76
76
35. 76
35. 76
35. 76
35, 76
35, 76
35
35
30. 35. 76


References [1]
35, 76
35, 76
35. 76
35. 76
35. 76
35, 76
76
76
35
35
30, 76
iltMArfl* A frM
Mono-CB
01-CB
TM-CB
Tttra-CB
Penta-CB
Hexa-CB
Htpta-CB
Octa-CB
Nona-CB
Dtca-CB

TOTAL PCBS
NO  - Not Otttcttd: tht dttt«
[1] - Tht nu0btr(s) In tht n
      which tht conctntratlon rangt froa prtvlous studies MU extracted.
[2] - Tht conctntratlon rangt* wtrt derived froa both coetolntd bottpi/fly and discrete  botton ash  sanples.
                                                 5-4

-------
      The concentration ranges for PCDDs  and PCOFs  in fly  ash  and combined
 ash are presented in Table 5.3.   This  table shows  that  both the fly ash
 and combined ash results  for PCDDs and PCOFs generally  exceed the
 'concentration ranges from the previous studies,  particularly  for the
 highly chlorinated species of both PCDDs and PCDFs (i.e.,  the hexa-
 through octa-chlorinated  species  of both PCDDs and PCDFs).  These
 exceedances  are  more pronounced for the  PCDDs than for  the PCDFs.
 Similarly, they  are more  pronounced for  the fly  ash than  for  the combined
 ash.   These  discrepancies may again be explained by the lack  of a
 complete data  base  from previous  studies.
      5.1.2   Laboratory Leachates
      Table 5.4 presents the  concentration  ranges for metals in the EF
 (extraction  procedure  toxicity) leachates  prepared from fly ash and
 combined ash samples.   The results for the EP-prepartd  fly ash leachates
 from  this study  are  within the concentration ranges from  previous
 studies,  except  for  iron  and manganese,  where slightly  higher results
 were  found by  Ve-rsar.   Similarly,  the  results for. the EP-prepared
 combined ash leachates  from  this  study are within  the concentration
 ranges from previous studies  for  all metals except copper, iron, lead,
 and zinc.  As  was the case for the solid samples,  these slight
 discrepancies  may be attributed to the concentration ranges which were
 extracted from one previous  study of only  one MWC  facility.
     The concentration  ranges for metals in the  TCLP (toxicity charac-
 teristic leaching procedure)  leachates prepared  from fly  ash  and combined
 ash samples are given in  Table 5.5.  Although the  cadmium, copper, lead,
 and nickel results £torn the Versar study are  within the concentration
 ranges from the previous  studies,  the  results for  the TCLP-prepared fly
 ash leachates from this study are  generally higher than the upper end of
 the ranges from the previous studies.  Similarly,  the results for the
TCLP-prepared combined ash leachates from  this study exceeded the upper
end of the ranges from previous studies  for cadmium,  chromium, manganese.
                                    5-5

-------
                     TABLE 5.3  COMPARATIVE EVALUATION OF PCOO/PCOFs IN SOLID SAMPLES
                                                 FLY ASH
Conetntratlon
PCOO/PCOF Homo log
2,3.7.8-TCDO
Tetra-CDO
Penta-COO
Hexa-CDO
Htpta-COO
Octa-COO
TOTAL PCOOs
2.3.7.8-TCOF
Tetra-COF
Penta-COF
Htxa-COF
Htpta-COF.
Octa-COF
This Study
0.
2




64
11 -
.3 -
a -
18 -
14 -
11 -
.3 -
Rangt Fro»
(ng/g)
3.9
43
722
5.565
3,030
3,152
10.883
It.A.

7

3
1
20 -
.1 -
14 -
.8 -
.4 -
169
226
2.353
666 .
362
Conetntratlon
Prtvlous
N0(0

Rangt Fro»
Studies (ng/g)
.
2
1) -
.4 -
0.5 -

N0(0
N0(0
N0(0
N0(0
0
•
•
•
•
.2 -
1) -
1) -
1) -
1) -
0.4 -
N0(0.
. ND(0.
N0(0
N0(0
*
•
1) -
1) -
1) -
1) -
42
250
650
2.496
410
341.5
4,700
5.4
460
1,800
1,100
500
255



References
30

35
12

12
12. 30

35
35


12

76
f
,
76
»
»
76
f
*
76
76
,
76

76
76

76
35.

76
76


76

[13






76






TOTAL PCOFs
60.2 - 3,187
NO(O.l) - 3,000
                                                       30.  76
TOTAL PCOO/PCOFs
124.5 - 14.070
                           NO(O.l)  -  7,700
                       12. 30, 35, 76
                                             COMBINED ASH [2]
I «

PCOO/PCOF Homo log
2.3.7,8-TCOO
Tttra-COO
Ptnta-COO
Htxa-COO
Htpta-COO
Octa-COO

Conetntratlon Rangt Fro»
This Study (ng/g)
NO(O.l) - 0.78
NO(O.l) - 14
NO(O.l) - 50
NO(O.l) - 78
NO(O.l) - 120
0.16 - 89

Conetntratlon Rangt Frot
Prtvlous Studies (ng/g)
0.2 - 6.7
0.13 - 92
NO(O.l) - 13
NO(O.l) - 9.0
NO(O.l) - 1.7
NO(O.l)


References [1]
76
76
35. 76
35. 76
35. 76
35. 76
TOTAL PCOOS
0.27 - 350
NO(O.l) - 110
                                                     30. 35, 76
                                                  5-6

-------
                                          TABLE S.3  (CONTINUED)


                                             COMBINED ASH [2]
                                 Concentration Range Fro»      Concentration Range Fnm
PCDO/PCOF Homolog                   This Study (ng/g)          Previous Studies  (ng/g)     References  [1]
2.3.7.8-TCDF                         ND(O.l) - 12                      0.2 -  1.3                76
Tetra-COF                            NO(O.l) - 91                  NO(O.l) -  8.4                76
Penta-COF                            NO(O.l) - 37                  NO(O.l) -  12                 76
Hexa-COF                             NO(O.l) - 35                  NO(O.l) -  2.5              35,  76
Hepta-COF                            NO(O.l) - 36                  NO(O.l) -  0.8              35,  76
Octa-COF                             NO(O.l) - 8.4                 NO(O.l) -  0.9              35.  76

TOTAL PCOFs                             0.18 - 153.9               NO(O.l) -  65             30,  35,  76


TOTAL PCOO/PCOFs                        0.48 - 480.4               NO(O.l) -  175            30,  35,  76
N.A.- Not Available
NO  • Not Detected; tne detection Halt Is given In parentheses following NO.
[1] - The nui*er(s) In the reference column corresponds to the reference Item number in Appendix A from
      which the concentration range from previous studies wes extracted.
[2] • The concentration ranges were derived from botn combined bottom/fly and  discrete bottom ash samples.
                                                 5-7

-------
                        TABLE S.4  COMPARATIVE EVALUATION  OF METALS IN EP LEACHATES
                                                 FLY ASH
 Metal
Arsenic  (As)
Cadmium  (Cd)
Chromium (Cr)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury  (Hg)
Nickel (N1)
Selenium (Se)
Zinc (Zn)
Metal
Arsenic (As)
Cadmium (Cd)
Chromium (Cr)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Nickel (N1)
Selenium (Se)
Zinc (Zn)
Concentration Range From
This Study (mg/L)
NO(O.Ol)
6.02 - 18.0
NO(O.OOS) - 0.038
0.041 - 1.62
N0(0.005) - 0.49
4.72 - 25.2
2.71 - 8.03
MO (0.008)
0.137 - 1.92
NO(O.OS)
188 - 728
COMBINED ASH [2]
Concentration Range From
This Study (rag/L)
NO(O.Ol)
0.06 . 0.827
0.0059 - 0.150
0.039 • 1.19
4.S • 143
2.09 - 34
3.60 • 5.24
N0(0.008)
0.241 . 0.415
N0(0.05)
38.5 - 726
Concentration Range From
Previous Studies (ng/L)
NO(O.OOl) - 0.858
0.025 . 100
0.006 - 0.135
0.033 - 10.5
0.189 - 0.202
0.019 • 53.35
0.005 - 5.79
N0(0.0002) • 0.007
0.09 . 2.90
H0( 0.002) - 0.085
3.36 • 768

Concentration Range From
Previous Studies (ng/L)
NO(O.OOl) .0,122
0.018 - 3.94
K0(0.007) - 0.46
0.713 - 0.898
94.3 - 96.5
0.02 - 21.0
5.62 - 6.21
N0(0.0002) - 6.00
0.463 - 2.03
N0(0.002) • 0.10
64.5 - 81

References [1]
30. 53
42. S3
30. 53
53
53
30, 53
53
30, 53
53
30, 53
53


References [1]
30, 53
30, 53
30, 53
53
53
53
53
30. 53
53
30. 53
53
NO  ' Not Detected; the detection limit Is given In parentheses  following NO.
[1] ' The numbers) in the reference column corresponds  to the reference  item number  1n Appendix A  from
      which the concentration range from previous studies MS extracted.
[2] ' The concentration ranges were derived from both combined bottom/fly and discrete bottom ash samples.
                                                  5-8

-------
                        TABLE  5.5   COMPARATIVE EVALUATION OF HETALS IN TOP LEACHATES
                                                 FLY ASH
 Metal
Arsenic  (As)
Cadmium  (Cd)
Chromium (Cr)
Copper (Cu)
Iron  (Fe)
Lead  (Pb)
Manganese  (Mn)
Mercury  (Hg)
Nickel (N1)
Selenium (S«)
Zinc  (Zn)
Concentration Range Fr
   This Study (ng/L)

   NO(O.Ol) - 0.111
      0.015 - 17.2
  NO(0.005) - 0.544
  NO(O.OOS) - 0.201
  NO(O.OOS) - 190
   NO(O.OS) - 15.2
      0.049 - 14.7
        NO(O.OOS)
  N0(0.015) - 1.52
        NO(O.OOS)
      0.151 • 746
Concentration Range From
Previous Studies (ng/L)
References [1]
            N.A.
        0.03 • 20.3
        0.02 • 0.12
        0.02 - 14.7
        0.03 - 0.17
         5.3 • 36.6
        0.01 > 7.19
            N.A.
        0.09 - 2.48
            N.A.
       •2.27 - 8.85
      N/A
      S3
      S3
      53
      53
      S3
      S3
      N/A
      S3
      N/A
      53
                                             COMBINED ASH [2]
Metal
Arsenic (As)
Cadmium (Cd)
Chromium (Cr)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Nickel (Nl)
Selenium (Se)
Zinc (Zn)
Concentration Range From
This Study (ng/L)
NO(O.Ol) - 0.037
0.025 • 3.32
NO(O.OOS) • 0.439
NO(O.OOS) - 0.019
0.828 - 60.6
0.655 - 30.1
4.2 • 11.9
N0(0.008)
0.344 - 0.805
NO(O.OOi)
23.3 • 373
Concentration Range From
Previous Studies (ng/L)
0.01
0.01
0.01
0.02
2.18
0.05
3.22
N0(0.0002)
0.09
0.01
23.5
- 0.1
. 1.9
- 0.32
- 0.09
- 230
• 47
- 7.47
• 0.10
. 0.41
. 0.05
- 83.2
References [1]
53
S3
S3
53
S3
S3
S3
S3
53
S3
53
N.A.- Not Available; N/A - Not Applicable
NO  - Not Detected: the detection limit Is given In parentheses following NO.
[1] - The numoer(s) In the reference column corresponds to the reference Item number In Appendix A from
      which the concentration range from previous studies MM extracted.
[2] - The concentration ranges were derived from both combined bottom/fly and discrete bottom ash samples.
                                                  5-9

-------
 nickel, and zinc.   Again,  these  discrepancies may have been a  result of
 the limited amount of-data available  in previous studies.
      The concentration ranges  for  metals in deionized water leachates
 prepared from the  fly ash  and  combined  ash are presented  in Table 5.6.
 Special care should be taken when  comparing and evaluating the data in
 this table because the monofilled  waste extraction procedure (MWEP;
 SW-924) was used by Versar,  but  the nature of the deionized water
 leaching procedure used in the previous study is not known.
 Nevertheless,  Table 5.6 shows  that the  concentrations from this  study for
 both the fly ash and combined  ash  are comparable to the concentrations
 from previous  studies.
      5.1.3  Field  Water Samples
      The concentration ranges  for  metals in field leachate and quench
 water samples  are  presented  in Table 5.7.  The field leachate  results
 from this  study  are within the concentration ranges from  the previous
 studies .for every  metal.   Generally, the concentrations from this study
•are  in  the lower end of the  concentration ranges from previous studies.
 Conversely,  the  quench water concentrations from this study exceed  the
 upper boundary of  the ranges from  previous studies for metals.   One
 possible  explanation for this  is that several of the quench water samples
 from this  study  contained  appreciable amount of solids (i.e.,  ash
 material).   Since  total metals were quantified, the samples were
 subjected  to the acid digestion and subsequent analysis without  a
 filtration step.   AM  a  result, the quench water sample results may  have
 been biased high in comparison to  other studies by the solid materials.
 Nevertheless,  the  data  reported  in this study characterizes the  quality
 of the  waatewater  which is discharged.
      Table 5.8 presents the  concentration ranges for organic constituents
 (BNAs)  in  field  leachate and quench water samples.  Both  the field
 leachate and quench water  results  from  this study are generally  within
 the  concentration  ranges from  the  previous studies, where the  data  are
                                    5-10

-------
                  TABLE  5.6   COMPARATIVE EVALUATION OF METALS IN OEIONIZEO WATER LEAOATES
                                                 FLY ASH
 Metal
 Arsenic  (As)
 Cadmium  (Cd)
 Chromium (Cr)
 Copper (Cu)
 Iron  (Fe)
 Lead  (Pb)
 Manganese  (Mn)
 Hercury  (Hg)
 Nickel (141)
 Selenium (Se)
 Zinc  (Zn)
Concentration Range From
This Study (ng/L)
NO(O.Ol)
NO(O.Ol) . 0.122
NO(O.OOS) • 0.15
NO(O.OOS) - 0.089
NO(O.OOS) - 0.167
NO(O.OS) - 0.148
NO(O.OOl) . 0.0052
N0(0.02)
NO(O.OIS) - 0.022
NO(O.OOS) - 0.108
HO (0.003) . 1.22
COMBINED ASH [2]
Concentration Range From
Previous Studies (ng/L)
N.A.
0.03 - 0.17
0.04 . 0.08
N0(0.02)
N0(0.03)
0.26 - 35.0
NO(O.Ol)
N.A.
NO(O.OIS) - 0.09
. N.A.
0.67 - 4.15

References [1]
N/A
53
53
53
53
53
53
N/A
53
N/A
53

Metal
Arsenic (As)
Cadmium (Cd)
Chromium (Cr)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Nickel (N1)
Selenium (Se)
Zinc (Zn)
Concentration Range From
   This Study (mg/L)

        NO(O.Ol)
        NO(O.Ol)
        NO(O.OOS)
  NO(O.OOS) - 0.07
  NO(O.OOS) - 0.038
   NO(O.OS) • 0.063
  NO(O.OOl) - 0.0021
        N0(0.02)
        NO(O.OIS)
        NO(O.OOS)
  N0(0.003) - 0.067
Concentration Range From
Previous Studies (ng/L)
References [1]
         NO(O.OS)
        0.01 - 0.03
    NO(O.Ol) . 0.02
        0.11 - 0.19
         N0(0.03)
    ND(O.OS) - 2.98
         NO(O.Ol)
         NO(O.IO)
    N0(0.02) - 0.09
         NO(O.OS)
        0.38 - 0.96
      53
      53
      53
      53
      53
      53
      53
      53
      S3
      53
      53
N.A.- Not Available; N/A - Not Applicable
NO  • Not Detected; tiw detection limit Is given In parentheses following NO.
[1] - The number(s) In the reference column correspond! to tne reference item matter In Appendix A fro*
      which the concentration rang* from previous studies MM extracted.
[2] - The concentration ranges were derived from both combined bottom/fly and discrete bottom ash samples.
                                                 5-11

-------
                  TABLE  5.7   COMPARATIVE EVALUATION OF TOTAL NETALS IN FIELD WATER SAMPLES
                                             FIELD LEACHATE
 Metal
Arstnlc  (As)
Cadmium  (Cd)
Chromium (Cr)
Copper (Cu)
Iron  (Fe)
Lead  (Pb)
Manganese (Nn)
Mercury  (Hg)
Nickel (N1)
Seleniua (S«)
Zinc  (Zn)
Concentration Range Froai
   This Study («g/L)
NO(O.Ol)
NO(O.OOS)
NO(O.QOS)
0.045
0.758
NO(O.OS)
0.103
N0(0.0002)
NO(O.OIS)
NO(O.OOS)
0.048
- 0.218
• 0.044
• 0.914
- 2.57
- 121
- 2.32
• 4.57
• 0.008
- 0.412
• 0.037
• 3.30
                        Concentration Range Fro*
                        Previous Studies (ng/L)
                         References [1]
NO(O.OS)
NO(O.Ol)
N0(0.006)
N0(0.006)
«( 0.007)
NO(O.OOl)
N0( 0.002)
N0(0.002)
NO(O.OS)
N0(0
NO(O.Ol)
- 70.2
- 17.0
- 33.4
- 24.0
- 5,500
- 14.2
- 1,400
- 0.064
- 7.5
.01)
• 1,000
30. 52
30, 52
30, 52. 69
30. 52
30, 52, 69
52
52
30, 52
30. 52
30
30, 52
                                              QUENCH HATER
Metal
Concentration-Range Fro*
   This Study (rag/L)
Arsenic (A$)
Cadmium (Cd)
Chrc«1u») (Cr)
Cooper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Nickel (Ni)
Selenium (Se)
Zinc (Zn)
   NO(O.Ol)
  NO(O.OOS)
     0.0085
       0.02
      0.037
      0.178
      0.024
 N0(0.0002)
      0.009
        0.542
        1.91
        1.12
        13.1
        141
        37.9
        12.6
        0.022
        0.849
  10(0.0125)
0.087 . 192
                        Concentration Range From
                        Previous Studies (mg/L)
                         References-[1]
 NO(O.OOl) .
 110(0.004} •
 10(0.007) •
       N0(0,
       N0(0.
 NO(O.OOl) •
       N0(0.
N0(0.0002) •
       N0(0,
 (€(0.002) .
       N0(0
 0.0031
 0.067
> 0.014
006)
007)
 0.688
002)
• 0.0089
015)
> 0.036
002)
46, 56
46. 56
46, 56
  46
  46
46, 56
  46
46, 56
  46
46. 56
  46
NO  - Not Detected: the detection llartt ts given (a parentheses following NO.
[1] - The nueoer
-------
                      TABLE 5.3  COMPARATIVE EVALUATION OF BNAs IN FIELD  MATER SAMPLES
                                             FIELD LEACHATE
 SKA Conpound
 Biphtnyl
 01-n-butyl  phthalata
 01ethyl  phthalate
 Dimethyl  phthalate
 Dimethyl  propanedlol
 Bis 2-ethylhexyl phthaiate
 Naphtha lent
 Phenol
 Thlolant
SNA Compound
Acenaphthylene
Benzole add
01-n-butyl phthai ate
Bis 2-ethylhexyl phthaiate
Fluoranthene
Hexanolc add
2-Hydroxybenzolc acid
Methylpentanolc add
2-Methyl phenol
4-Metnyl phenol
Naphthalene
Phenanthrene
Phenol
Pyrene
Concentration Range Fro*
This Study (ug/L)
NO(N.A.) - 51
N0(2.5)
N0(22)
NOU.6)
NO(N.A.) . 120
N0(2.5) - 80
N0(1.6)
NO(l.S)
NO(N.A.) - 400
QUENCH MATER
Concentration Range Froai
This Study (ug/L)
110(3.5) - 6.0
NO(N.A.) - 3,800
N0(2.5) • 3.0
N0(2.5) - 8.0
N0(2.2) • 6.0
NO(N.A.) . 920
NO(N.A.) - 50
NO(N.A.) . 88
N0(2.7) - 86
N0(2.7) - 94
NOU.6) . 8.0
N0(5.4) . 6.0
NO(l.S) - 640
N0(1.9) - 5.0
Concentration Rang* Fron
Previous Studies (ug/L)
N.A.
N0(2.5) - 150
N0(2.2) - 300
N0(1.6) - 55
N.A.
N0(2.5) - 150
N0(1.6) - 19
N0(1.5) - 29,800
N.A.

Concentration Range Fro*
Previous Studies (ug/L)
0.46 - 28
N.A.
N0(0.6) - 13
N0(0.6) - 1.3
0.45 • 1.5
N.A.
N.A.
N.A.
N.A.
N.A.
N0(0.6) - 3.0
N0(0.6) • 5.0
N.A.
0.57 - 4.4

References [1]
N/A
52
52
52
N/A
52
52
52
N/A


References [1]
35
N/A
35
35
35
N/A
N/A
N/A
N/A
N/A
35
35
N/A
35
N.A.. Not Available; N/A - Not Applicable
NO  - Not Detected: the detection Malt  is given  in parentheses following NO.
[1] - The nunber(s) In the reference coluen  corresponds to the reference Itea
      which the concentration range fro* previous studies MU extracted.
In Appendix A fro»
                                                5-13

-------
 available.  The  results of both this study and the previous studies
 indicate  that the polycyclic aromatic hydrocarbons (e.g., acenaphthylene,
 fluoranthene, naphthalene, phenanthrene, and pyrene), the phthalate
 esters  (e.g.. bis-2-ethylhexyl phthalate, di-n-butyl phtnalate, diethyl
 phthalate, and dimethyl phthalate), and the phenols (e.g., phenol, methyl
 phenol, and dimethyl phenol) are the predominant SNA compounds that were
 detected  in the  field water samples.
     5.2  Significant Trends in the Data from this Study
     The data generated from the samples collected in this study were
 summarized by facility and sample type (e.g., ground water, field
 leachate, fly ash, combined ash EP leachate, etc.) to facilitate data
 evaluation.  The data summaries were generated by averaging the
 individual analytical results for each sample type from each facility.
 One summary was prepared for the metals data, and another one was
 prepared for the PCBs, PCOOs, and PCDFs.  A summary was not prepared for
 the BNAs because very few of the individual SNA constituents were
 detected often enough to allow for a meaningful comparative evaluation.
     5.2.1  Metals
     The summary of the metals data is presented in Table 5.9.  The
metals data for the solid samples showed that the fly ash contained more
 total metals than the combined (i.e., bottom/fly) ash or the bottom ash.
The fly ash consistently exhibited higher concentrations o£ cadmium,
chromium, lead, nickel, zinc, arsenic, mercury, and selenium than the
combined ash or bottoo ash.  However, the combined ash and bottom ash
contained higher concentration* of copper and iron.  The fly ash
contained approximately the same, amount of manganese as the combined  ash
and bottom ash.  These observations suggest that the which tend to become
more concentrated in the fly ash are the more volatile metals, while
those metals that are more highly concentrated in the combined ash and
bottom are the higher boiling point less volatile metals.
                                   5-14

-------
                                            TABLE 5.9  SUMMARY RESULTS FOR METALS
                                                          FACILITY A
Sanplt
Typt
Fly Ash
Fly Ash
Fly Ash
Fly Ash
Fly Ash
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Bottom/Fly
Samp It
Matrix
Solid
EP Tox.
TCLP
SW924-EX1
SW924-EX2
Solid
EP Tox.
TCLP
SW924-EX1
SW924.EX2

units
mg/kg
«g/L
mg/L
mg/L
mg/L
mg/kg
mg/L
mg/L
mg/L
mg/L

Cd
190.8
6.37
0.023
<0.015
<0.01
19.3
0.827
0.682
<0.01
<0.01

Cr
70.3-
<0.005
0.136
0.01
<0.005
16.3
0.016
0.096
<0.005
<0.005

Cu
1716
0.15
<0.005
0.058
0.009
356
1.19
0.019
<0.005
<0.005

Ft
15646
<0.005
190
0.167
0.057
5904
4.50
60.6
<0.005
<0.005

Pb
5636
7.76
0.962
<0.075
0.072
1246
20.3
16.3
<0.05
«0.005

Mn
997
7.32
2.33
0.004
0.003
247
4.15
7.18
<0.001
<0.001

HI
110
0.396
0.372
0.0225
<0.015
22.0
0.241
0.346
<0.015
<0.015

Zn
14436
224
38.9
0.036
0.083
2010
38.5
55.8
<0.003
0.0031

AS
36.3
-0.01
0.024
<0.01
<0.01
6.3
<0.01
0.020
<0.01
<0.01

Hg
26.3
<0.008
<0.008
<0.04
<0.02
6.3
<0.008
<0.008
<0.02
<0.02
  Quench       Wattr    •mg/L




Groundwattr    Wattr    mg/L
  0.09    0.016    0.185    1.48   5.005   0.1355   0.009   5.475   0.011  0.0117    O.i




<0.005   0.0067   0.0086    2.39  <0.050    0.107  <0.018   0.029  <0.010 <0.0002   <0.
                                                          FACILITY 8
Samp It
Typt
Fly Ash
Fly Ash
Fly Ash
Fly Ash
Fly Ash
BottM Ash
BottM Ash
BottM Ash
BottM Ash
BottM Ash
Field Ltachatt
Qutnch
Groundwtttr
Samp It
Matrix
Solid
EP Tox.
TCLP
SW924-EX1
SW924-EX2
Solid
EP Tox.
Tap
SW924-EX1
SH924-EX2
Wattr
Wattr
Wattr

Units
mg/kg
mg/L
mg/L
•g/L
mg/L
«g/kg
•g/L
•g/L
•g/L
•g/L
•g/L
mg/L
mg/L

Cd
349
18
17.2
<0.01
0.033
10.74
0.388
0.418
<0.01
«0.0l
0.018
0.0025
0.0081

Cr
94.3
•cO.OOS
<0.005
0.0086
0.01
61.2
0.15
0.439
<0.005
<0.005
0.0097
0.019
0.0054

Cu
765
0.171
0.078
<0.005
0.012
4209
0.127
0.018
0.0089
«0.005
0.0973
0.0363
0.012

Ft
12742
0.060
0.019
«O.OOS
0.118
39140
21.0
52.8

-------
TABLE 5.9   SUMMARY RESULTS FOR METALS
              FACILITY C
Sample Sample
Type Matrix
Fly Ash Solid
Fly Ash EP Tox.
Fly Ash TaP
Fly Ash SW924-EX1
Fly Ash SW924-EX2
Bottom/Fly Solid
Bottom/Fly EP Tox.
Bottom/Fly TCLP
Bottom/Fly SW924-EX1
Bottom/Fly SU924-CX2
Perimeter Comp. Solid
Field Leachate Water
Quench . ... Water. .
Groundwater Water

Sample Sample
Type Matrix
Fly Ash Solid
Fly Ash EP Tox.
Fly Ash TaP
Fly Ash SW924-EX1
Fly Ash SU924-EX2
Bottom/Fly Solid
3otton/Fly EP Tox.
Bottoei/Fly TaP
SottOM/Fly SW924-EX1
Bottoa/Fly SW924-EX2
Perimeter Coop. Solid
Field Lwcnate water
Quench Water

units
mg/kg
mg/L
mg/L
mg/L
mg/L
mg/kg
mg/L
mg/L
mg/L
mg/L
mg/kg
mg/L
mg/L..
mg/L


Units
mg/kg
mg/L
mg/L
mg/L
mg/L
•J/kg
mg/L
mg/L
mg/L
mg/L
mg/kg
mg/L
mg/L

Cd
173.2
7.89
3.36
0.122
-0.01
17.8
0.06
3.32
<0.01
<0.01
8.7
0.0117
0.128
<0.010


Cd
226.6
8.89
9.6
0.015
<0.01
24.2
0.649
0.025
<0.01
<0.01
30
0.0188
1.335

Cr
55.8
0.038
0.129
0.006
<0.005
87.2
0.0059
<0.005

-------
      The analytical results for the metals in the landfill perimeter
 composite were expected to approximate the results for the combined ash
 samples from the corresponding facilities.  Although some slight
 variations were noted, the data in Table 5.9 showed that the metals
 concentrations for the perimeter composite and combined ash samples were
 approximately equal.  The slight variations can be attributed to the
 effects of weathering on the older ash, the heterogeneity of the ash
 materials, and the variability of the raw refuse that is incinerated at
 the facility.   These observations suggest that the amount of leachable
 metals present in the disposed ash is a relatively small percentage of
 the total  metals.
      The quench water at all four facilities is discharged to the local
 publicly owned treatment works (POTW).   In general,  the analyses of the
 quench water samples indicated that the quality of the quench water was
 suitable for discharge to a POTW.   However,  the quench water from
 Facility 0 had extremely high concentrations of metals because the
 samples  were collected from the quench  water tank and contained an
 appreciable  quantity of solid materials.
      Field leachate  samples were collected from natural seeps at three
 facilities of  the  four facilities  tested.   The leachate discharges are
 not controlled  or  treated at  any of the facilities.   Therefore,  they
 eventually percolate  into the  ground or flow into nearby surface waters.
 The field  leachate data in Table S.9 showed  that the  metals
 concentrations  at all  three facilities  were  essentially equal,  despite
 the fact that the solid samples  of  the  ash materials  disposed at the
 three landfills contained  significantly different metals concentrations.
 This suggests that the  leachable metal  components in  the ash do not vary
 in direct proportion with  the  total  metals concentration.
     A comparison of the metals  concentrations in the quench water and
 field leachate showed that  the field leachates generally contain slightly
higher concentrations of metals.  This  suggests  that  the metals leach
                                   5-17

-------
 slowly from the landfills  at  a  relatively constant rate, and that they
 usually are not leached in the  quench water tank.
      The laboratory-prepared  leachate metals data in Table 5.9 indicated
 that the EP and TCLF  methods  are more aggressive for extracting metals
 than the SW-924 procedure.  This was expected because an acidic leaching
 solution is used for  both  the EP and TCLP methods, while in the SW-924
 procedure,  a neutral  leaching solution  (i.e., deionized water) is used.
 The  EP  and  TCLP procedures  appeared to  have approximately equal
 extraction  efficiencies  for cadmium, copper, iron, nickel, zinc, mercury,
 and  selenium.   The EP method  appeared to extract lead slightly more
 efficiently than the  TCLP method, but the TCLP method appeared to be
 slightly more efficient  for extracting  arsenic, chromium, and manganese.
     Upon comparing the  laboratory leachate metals data for the fly ash
 with the  combined ash and bottom ash, the following trends were noted.
 Although  the fly ash  solids contained higher concentrations of cadmium,
 chromium, lead,  nickel,  and zinc than the combined ash and bottom ash
 solids,  the  fly ash leachates contained higher concentrations than the
 combined  ash and bottom  ash leachates for cadmium.  This suggests that
 the leachable fractions  of  chromium, lead, nickel, and zinc are inherent
 in the bottom ash.  Similarly,  the combined ash and bottom ash solids
 exhibited higher  concentrations of copper and iron than the fly ash
 solids.  However, the combined  ash and  bottom ash leachates contained
 higher concentrations than  the  fly ash  leachates for iron.  This
 indicates that  the component of the total 'copper is inherent in the fly
 ash.   Finally,  the total manganese concentrations were approximately
 equal for the fly ash solids and the bottom ash and combined ash solids;
 however, the combined ash and bottom ash leachate contained slightly
 higher manganese concentrations than the fly ash leachates.  Therefore,
 the leachable fraction of manganese appears to be inherent in the bottom
 ash.
     A comparison of the metals concentrations in the field leachates
with those in the laboratory-prepared leachates showed that the EP and
                                   5-18

-------
 TCLP methods approximated the natural  leaching  conditions  for  chromium,
 copper, iron, nickel,  arsenic, mercury,  and  selenium  better  than  the .
 SW-924 procedure.   Conversely, the SW-924  procedure appeared to better
 correlate with the natural leaching conditions  for cadmium,  lead,
 manganese, and zinc.
      For the ground-water metals  data, the concentrations  were generally
 negligible for all metals except  iron.   Therefore, it does not appear
 that the natural field leachate is having  a  deleterious  effect on the
 ground water.   However,  no ground-water  data were available  to describe
 background (i.e.,  upgradient  from the  landfill) conditions.  At each
 facility,  with the possible exception of Facility C,  the quality  of the
 monitoring wells systems including the design and locations  of the
 monitoring wells may not have  been adequate  to  detect releases from the
 landfill areas.  Therefore, the actual magnitude of the natural
 leachate's  effect  on the ground water could  not be discerned.
      5.2.2   Polychlorinated Biphenyls, Polychlorinated Dibenzo-p-dioxins,
             and Polychlorinated Dibenzo-furans
      The analytical results for the PCBs,  PCDDs, and  PCOFs are summarized
 by facility in Table 5.10.  The PCS, PCDD, and  PCOF results  for the solid
 samples  showed that the  fly ash consistently contained higher  concentra-
 tions of PCBs, PCDDs,  and PCDFs than the combined ash and  bottom  ash.
 The data also showed that  the  PCDDs were generally more concentrated than
 the PCDFs and the  PCBs in all  sample types.  Similarly, the  PCDFs  were
 much more concentrated than the PCBs for all sample types;
     The field water sample results indicated that negligible  quantities
 of PCBs were present in  these  matrices,  and  only minor quantities of PCDDs
 and PCDFs were identified.  This  suggests  that  the PCBs, PCDDs, and PCDFs
 are not mobile in  the natural  environment  through aqueous  transport
 pathways.  The PCDD and  PCDF results for the TCLP- prepared  laboratory
 leachates were not presented in Table 5.10 because they were generally
near, or below, the detection  limit.  This suggests that the TCLP does
not extract PCDD and PCDF constituents effectively.
                                   5-19

-------
TABU  S.10  SUMMttY RESULTS FOR PC3*. OIOXINS AND FURAHS
Plant
A
A
A

Plant
A
A
A
A
A
A

Plant
8-
3
3
8

Plant
B
3
8
a
a
a
a
a
Sa*ple
Type
Fly Ash
Bottom/Fly
Quench
Sanple
Typt
Fly Ash
Fly Ash
3otton/F1y
3ottan/Fly
Quench
Quench
Sample
Type
Fly Ash
Bottom Ash
Quench
Field Leachate
Sane I «
Type
Fly Ash
Fly Ash
Sottoai Ash
Bottom Ash
Quench
Quench
Field Leachat*
Field Leachat*
Suple
Matrix
Solid
Solid
Water
Sanple
Matrix
Solid
Solid
Solid
Solid
water
Water
Sanple
Matrix
Solid
Solid
Water
water
Sample
Matrix
Solid
Solid
Solid
Solid
water
water
Water
Water
Units
ng/g
ng/g
ug/L

Units
ng/g
ng/g
ng/g
ng/g
"9/1
ng/1

Units
ng/g
ng/g
ug/L
ug/L

Units
ng/9
ng/g
ng/g
ng/g
ng/1
ng/1
ng/1
ng/1


Species
Oloxln
Furan
Oloxln
Furan
Oloxln
Furan







Species
Oloxln
Furan
Oloxln
Furan
Oloxln
Furan
Oloxln
Furan
MONO
-CB
0.64

2,3,7,3
0.16

0.14
5.09
<0.08
2.1
MONO
-CB
0.40

0.03


2.3.7.8
0.35

0.03
0.10
<0.07
<0.08
0.28
3.7
01
-CB
0.73
0.66
0.004

TETRA
4.32
43.6
5.57
39.10
2
12
0!
-CB
1.19




TCTTU
10.90
80.4
0.17
0.49
«0.07

-------
TABLE  5.10  SUMMftY RESULTS FOR PCBs. OIOXINS AND FURANS
Plant
C
C
C
C
C
C

Plant
C
C
C
C
C
C
C
C
C
C

Plant
0
0
0
0
0

Plant
0
D
0
0
0
0
0
0
0
0
Sarnie
Typt
Fly Ash
Bottom/Fly
Perimeter Comp.
Quench
Field Leachate
GroundMtar
Sample
Typt
Fly Asn
Fly Asn
Bottoa/Fly
Botton/Fly
Ptrlmttr Com.
Ptrlmttr Coop.
Quench
Qutncn
Fit Id Leachate
Fit id Ltachatt
Sample
Typ«
Fly Asn
Bottm/Fly
Ptrlmttr Coop.
Qutncn
Fitld Ltachate
Sample
'too
Fly Ash
Fly Asn
8ottO«/Fly
Botton/Fly
Ptrlmttr Com.
Ptrlmttr Com.
Qutncn
Qutncn
Fit Id Ltacnatt
Fitld leacnatt
Sam It
Matrix
Solid
Solid
Solid
water
water
water
Sample
Matrix
Solid
Solid
Solid
Solid
Solid
Solid
water
water
Hater
water
Sample
Matrix
Solid
Solid
Solid
water
Water
Samlt
Matrix
Solid
Solid
Solid
Solid
Solid
Solid
Water
Hater
Hater
Hater
Units
ng/g
ng/9
ng/g
ug/L
ug/L
ug/L

Units
ng/g
ng/g
ng/g
"9/9
ng/g
ng/g
ng/1
ng/1
ng/1
ng/1
-
Units
ng/g
ng/g
ng/g
ug/L
ug/L

Units
"8/9
ng/g
ng/g
ng/g
ng/g
ng/g
ng/1
ng/1
ng/1
ng/1


Species
Oloxin
Furan
Oloxin
Furan
Oloxin
Furan
Oloxin
Furan
Oloxin
Furan








Species
Oloxin
Furan
Oloxin
Furan
Oloxin
Furan
Oioxin
Furan
Oloxin
Furan
MONO
-CB
0.02

2.3,7.8
1.95
13.3
0.36
1.79
0.07
0.51
<0.31
0.55
1.6
11
MONO
-C3
0.94





2,3,7,8
0.54

0.07
0.56
0.15
1.3
17
99
<0.26
0.4
01
-CB
0.65
41.5
0.002

TETRA
27.2
102
6.50
11.42
1.2
2.4
0.59
2.4
28
65
01
-CB
4.00
0.71
0.689



TETRA
9.64
57.6
0.75
3.48
2.5
11
700
590
0.27
2.9
TRI
-CB
225

PENTA
500
152
25.8
12.50
5.7
3.9
5.9
4
93
64
TRI
-CB
3.91
6.52
2.36

0.008

PENTA
59.4
33
2.70
2.63
6
7.7
650
460
<0.22
2.4
TETRA
-CB
109

HEXA
2299
635
37.4
16.54
6.8
4
10
6.2
130
76
TETRA
-CB
2.48
16.50
1.54



HEXA
90.4
69.4
2.03
2.10
4.1
5.3
450
390
2.1
1.9
PENTA
-CB

HEPTA
1837
281
61.6
16.80
9
3.3
19
6.5
172
60
PENTA
-CB
2.25





HEPTA
50.0
47.6
1.95
1.34
4.2
2.7
420
280
8.3
1.2
TOTAL
PCB
0.65
0
375.5
0.02
0.002
0

OCTA
1782
128
44.3
4.08
6.1
0.31
12
1.4
120
15
TOTAL
PCS
11.41
3.42
4.589
0
0.008

OCTA
55.4
5.4
1.63
0.33
3.9
0.61
330
68
25
0.81


TOTAL
6445
1297
176
61.34
28.8
14.41
47.49
20.5
543
280








TOTAL
265
213
9.02
9.86
20.7
27.31
2550
1788
36.17
9.21

TCOO *
TCDF

7742

237

43.21

67.99

823-







TCDO «•
TCOF

478

13.38

43.01

4338

45.28
                    5-21

-------
      Two observations were noted from a comparison of the PCS, PCDD, and
 PCDF  results for all of the sample types.  First, there appeared to be an
 inverse relationship between the PCB and PCDD/PCDF concentrations (i.e.,
 as  the concentration for one of the constituents increased, the concentra-
 tion  for the other constituent decreased).  Second, the PCDOs and PCDFs
 appeared to be directly proportional (i.e., as the concentration for one
 of  the constituents increased, the concentration for the other constituent
 increased), although there did not appear to be any relationship between
 the relative abundance of either PCOOs or PCDFs in the total PCDD/PCDF
 concentration.  These observations suggest that the favorable conditions
 for PCDD and PCDF formation are similar, while the favorable conditions
 for formation of PCBs are unfavorable for the formation of PCDOs and PCDFs.
     5.3  Relationships Between Facility Design and Operating
          Characteristics and Contaminant Concentrations
     In this section, the trends observed in Section 5.2 were evaluated
with the facility design and operating characteristics in an attempt to
explain the trends.  Section 5.3.1 presents the evaluation for the metals
data,  and Section 5.3.2 presents the evaluation for the PCB, PCDD, and
PCDF data.
     5.3.1  Metals
     There did not appear to be any significant correlation between the
operating characteristics of the facilities and the metals concentrations
in the residue.  In general, the concentration of metal in the residues
is a function of the raw refuse (i.e., incinerator feed material)
composition.  Although the distribution of metals between the fly ash and
bottom ash did not appear to be a function of the facility operating
characteristics, it did appear to be influenced by design features of the
incinerator.  For example, a rotary kiln incinerator with refuse
processing (e.g., crushing or shredding) would be expected to have a
significantly higher concentration of metals in the fly ash than a
reciprocating grate incinerator without refuse processing.  This  is
expected because crushing or shredding reduce the particle size, and  the
                                   5-22

-------
 action of the rotary kiln results  in autogenous  grinding  (i.e.,  the
 attrition and impaction between the  particles),  which also causes  reduced
 particle size.
      5.3.2  Polychlorinated Biphenyls,  Polychlorinated Dibenzo-p-dioxins,
             and Polychlorinated Oibenzo-furans
      Comparisons between operating characteristics/facility design and
 PCS,  PCDD, and  PCDF  concentrations in the  residues  revealed the  following
 observations.   First,  the PCS  concentrations  in  both the  fly ash and
 bottom ash increased with decreasing incineration temperatures.  Second,
 the PCS concentrations were higher for  the water-wall grate incinerators
 (Facilities B and 0)  than for  the  other facility types.   Third,  both  the
 total PCDDs and the  individual  PCDD  homologs  increased in the fly  ash as
 the incinerator temperature increased.   Fourth,  no  correlations  were
 observed between the  facility  design and operating  characteristics and
 the bottom ash  concentrations  of PCDDs  or  PCDFs.  Finally, the PCDD and
 PCDF  concentrations  for both the fly ash and  the bottom ash were the
 highest  for the  combination rotary kiln/reciprocating grate facility
 (Facility C), and these concentrations  were the  lowest for the water-wall
 grate  facilities  (Facilities B  and D),  where  the concentrations  between
 facilities were  approximately  equal.
      5.4   Overall Assessment of Risk
     The  risks associated with  current  MWC facility practices were
 assessed  based on comparisons with applicable standards and criteria.
 Section 5.4.1 provides  the  comparisons  for the metals data.
 Section 5.4.2 presents  an evaluation of the risks associated with  the
 PCBs found in MWC residues.  Finally, Section 5.4.3 presents the risk
 assessment  for the PCDDs  found  in  MWC residues.
     5.4.1  Metals
     The  results of the fly ash and  combined  bottom/fly ash and  bottom
ash samples prepared by the  EP  and TCLP procedures  were compared to the
RCRA Maximum Allowable Concentrations for  arsenic,  cadmium, chromium.
                                   5-23

-------
 lead, mercury, and selenium.  The RCRA criteria for these six metals are
 as  follows:  arsenic =5.0 mg/L; cadmium =1.0 ng/L; chromium =5.0 cng/L;
 lead = 5.0 ng/L; mercury = 0.2 mg/L; and selenium = 1.0 mg/L.  Six fly
 ash samples were extracted using the EP method, and these leachates were
 analyzed for metals.  The results of these analyses (see Table 4.3)
 indicated that none of the samples were above the RCRA criteria for
 arsenic/ chromium, mercury, or selenium.  However, 100 percent (6 out
 of  6) of the EP fly ash leachates exceeded the RCRA criterion for
 cadmium.  The maximum cadmium concentration in an EP fly ash leachate was
 13.0 mg/L.  Similarly, 33 percent (5 out of 6) of the fly ash leachates
 failed the RCRA criterion for lead.   The maximum lead concentration was
 25.2 mg/L.
     Three combined ash and one bottom ash samples were prepared using
 the EP method and analyzed.  The results of these leachate analyses (see
Table 4.3) showed that all of the EP leachates were below the RCRA
criteria for arsenic, cadmium, chromium, mercury, and selenium.  However,
75 percent (3 out of 4} combined and bottom ash leachates exceeded the
RCRA criterion for lead.  The maximum lead concentration was 34.0 mg/L.
     The results for the TCLP-prepared leachates were similar.  For the
fly ash, 67 percent (4 out of 6) of the TCLP leachates exceeded the RCRA
criterion for cadmium, and 67 percent (4 out of 6) of the TCLP leachates
failed the RCRA criterion for lead.   The maximum TCLP leachate concentra-
tions for cadmium and lead were 17.2 mg/L and 15.2 mg/L, respectively.
The combined bottom/fly ash and bottom ash TCLP leachate results showed
that 25 percent (1 out of 4) of the leachates exceeded the RCRA criterion
for cadmium, and 75 percent (3 out of 4) of the leachates exceeded the
RCRA criterion for lead.  The maximum TCLP leachate concentrations for
cadmium and lead in the combined ash and bottom ash were 3.32 mg/L and
30.1 mg/L, respectively.  The metals concentrations in the TCLP  leachates
of fly ash, combined ash, and bottom ash were below the RCRA criteria for
arsenic, chromium, mercury, and selenium.  Additionally, the metals
                                   5-24

-------
 concentrations in the natural field leachates were below the RCRA
 criteria for all six metals.
      The analytical results for the ground-water samples metals
 concentrations (see Table 4.11) were compared to the  primary and
 secondary drinking water standards.  This  comparison  showed that all  of
 the ground-water samples contained concentrations significantly below the
 primary and secondary drinking water standards for all  metals except
 cadmium.   One ground-water sample  (monitoring well 2  at Facility B) had a
 cadmium concentration (0.0081 mg/L) that was  only slightly below the
 primary drinking water standard (0.01 mg/L).
      5.4.2  Pol/chlorinated Biphenyls
      The  EPA (TSCA)  classifies solid materials containing PCBs  as follows.
 If  the  solid material contains less than 50 parts per million (ppm) PCBs,
 it  is considered to  be non-hazardous and is not a regulated waste.  Solid
 materials  containing between  50 ppm and 500 pptn PCBs  must be handled  and
 disposed as  "PCB-containing"  materials.  Finally,  solid materials
 containing greater than 500 ppm PCBs must  be  handled  and disposed as
 hazardous  PCB .waste  materials.   The PCS analyses of fly ash,  bottom ash,
 and combined ash  (see Table 4.6) in this study showed that the  residues
 would not  be  regulated by TSCA based on their PCB content.   The maximum
 PCB concentration for a  fly ash sample was 24.77 ng/g (parts  per billion),
 and the maximum PCB  concentration for a bottom ash or combined  ash sample
 was 32.15  ng/g.  The  maximum  PCB concentration measured in this study was
 375.5 ng/g for a landfill perimeter composite  sample.   The field water
 samples contained negligible  concentrations of PCBs.
      5.4.3  Polychlorinated Dibenzo-p-dioxins
     The National Center for  Disease Control  has established a  level  of
 1.0 part per billion  (ppb) 2,3,7,3-TCDO in solid materials as the
acceptable limit.  The analytical results of  the solid  MWC residue
samples  for PCOOs (see Table  4.7) showed that  this  limit was occasionally
exceeded.   Twenty-seven percent  (6  out of 23)  of the  fly ash samples
                                   5-25

-------
contained 2,3,7,3-TCDD concentrations above 1.0 ppb, with a maximum
concentration of 3.9 ppb.  Therefore, these materials may be classified
as potentially hazardous wastes and should be treated accordingly.
Interestingly, all six of the samples exceeding the 1.0 ppb 2,3,7,3-TCDD
limit were collected at Facility C.  Although there are not any
established standards or criteria for total ?CDDs, several of the fly ash
samples (3 out of 22) had PCDO concentrations greater than 1,000 ppb
(1.0 ppb), with a maximum PCDD concentration of 12,013 ppb (12.0 ppm).
     The results for the combined ash, bottom ash, and landfill perimeter
composite samples were below the 1.0 ppb 2,3,7,8-TCDD limit, with a
maximum 2,3,7,3-TCDD concentration of C.78 ppb.  Similarly, the PCDO
concentrations for the field water and laboratory-prepared leachate
samples were negligible, with a maximum 2,3,7,3-TCDD concentration of
0.17 ppb and a maximum total PCDD concentration of 2.55 ppb.  This second
observation indicates that the PCDDs vigorously adhere to the solid
particles and are not mobile in the natural environment.
                                   5-26

-------
 6.0  CONCLUSIONS
      The objective of this study was to collect residues from four
 municipal waste combustor facilities for chemical characterization.  In
 order to meet this objective, a step-by-step approach was established.
 First, the four MWC facilities were selected based on the criteria
 described in Section 3.1.1.  Second, the facilities were visited, and the
 procedures detailed in Section 3.3 were used to collect the following
 samples:  fly ash, bottom ash or combined bottom/fly ash, disposed ash
 (i.e., landfill perimeter composite), quench water, ground water, and
 field  leachates.  Additionally, laboratory leachates were prepared from
 the fly ash and the bottom ash or combined ash samples using the EP,
 TCLP, and MWEP (SW-924)  procedures.  Third, these samples were analyzed
 for metals, PCBs,  PCOO/PCOFs, and organic constituents (i.e., total
 organic carbon,  organic scan, and BNAs) using the procedure* outlined in
 Section 3.4.   Finally,  the analytical data was compiled, summarized, and
 evaluated.   The  following conclusions were drawn from the results and
discussion presented in Section 4.0 and the evaluation provided in
Section 5.0.
      1.   The RCRA Maximum Allowable Concentration for cadmium was
          exceeded by 100 percent of the SP-prepared fly ash samples.
          However, the cadmium criterion was not exceeded by any of the
          EP-prepared combined ash or bottom ash leachates.
      2.   The RCRA Maximum Allowable Concentration for lead was exceeded
          by 83  percent of the EP-prepared fly ash leachates and by
          75 percent of the EP-prepared combined ash or bottom ash
          leachates.
      3.   The concentrations of metals in the ground-water samples did
          not exceed the primary or secondary drinking water standards.
          This suggests that the natural leachates from the landfill have
          not had  a major,  adverse impact on the ground water.
      4.   The PCS  concentrations were less than the 50 ppm limit
          established by TSCA for all solid samples.  Therefore, the
          solid  residues would not be classified as hazardous materials
          based  solely on their PCS content.
                                   6-1

-------
 5.  The 2,3,7,3-TCDD concentration exceeded the limit of 1.0 ppb
     established by the National Center for Disease Control in
     27 percent of the fly ash samples.  This limit was not exceeded
     by any of the combined ash or bottom ash samples.

 6.  The variability of the contaminant concentrations between days,
     shifts, and units at any given facility was significant,
     indicating that slight changes in the incinerator feed material
     (i.e., the raw refuse) and/or the operating parameters .
     significantly effected the quality of MWC residue.  The
     variability of the contaminant concentrations between the
     facilities was extremely large (i.e., the standard deviations
     of the concentrations exceeded the average concentrations).
     This suggests that the variability of operating characteristics,
     facility design, and feed material composition between
     facilities has a significant impact on the resultant MWC
     residue quality.

 7.  In general, the weight ratio of bottom ash to fly ash was
     approximately 3 to 1 for the four facilities in this study.

 8.  The quench water at all four facilities was discharged to the
     local wastewater treatment plant.  Based on the analytical
     results for the quench water samples, this appeared to be an
     acceptable disposal technique/ because uncontrolled discharges
     of quench water to the environment should be prevented.

 9.  None of the four facilities had a functioning leachate
     collection and/or treatment system.  However, the landfill at
     Facility A was designed and operated to minimize the contact
     between the waste and the environment, thereby reducing the
     potential for uncontrolled leachate discharges. ' The other
     three facilities did not control the discharges of natural
     field leachate.

10.  There did not appear to be any correlation between the operating
     characteristics of the facilities and the metals concentrations
     in the residues.

11.  The PCB and PCDD concentrations in the solid residues  increased
     with decreasing incinerator temperature.  Conversely,  the  PCDF
     concentration increased with increasing incinerator temperature.

12.  The PCB concentrations in the solid residues were the  highest
     for the water-wall grate incinerators (Facilities B and 0),  but
     the PCDD and PCDF concentrations were the highest for  the
     combination reciprocating grate/rotary kiln  incinerator
     (Facility C) and were lowest for the two water-wall grate
     facilities.
                               6-2

-------
 13.  The fly ash contained higher concentrations of all metals
     except copper and iron than the bottom ash.  Therefore.
     combining the ash fractions effectively diluted the total
     metals concentrations of the fly ash.

 14.  The fly ash consistently contained higher concentrations of
     PCBs, PCDDs, and PCDPs than the combined ash or bottom ash.
     However, the combined ash and bottom ash had higher
     concentrations of BNAs than the fly ash.

 15.  The concentrations of the predominant SNA compounds in the
     residues were generally near or below the detection limits.

 16.  The EP and TCLP methods were more aggressive than the MWEP
     (SW-924) method for extracting metals.  The EP method appeared
     to be slightly more efficient than the TCLP method for leaching
     lead; however, the TCLP method appeared to be slightly more
     efficient than the EP method for extracting arsenic, chromium.
     and manganese.  The extraction efficiencies of the EP and TCLP
     methods were approximately equal for the other metals.  None of
     the laboratory leaching procedures were efficient for extracting
     organic compounds.

 17.  The results of the EP and TCLP leachate analyses approximated
     the natural field leachate analytical results for chromium,
     copper, iron, nickel, arsenic, mercury, and selenium.  The
     SW-924 leachate concentrations for cadmium, lead, manganese,
     and zinc approximated the natural field leachate concentrations.

 18.  The leachable fraction of the total copper appeared to be
     inherent in the fly ash, and the leachable fractions of the
     total chromium, lead, manganese, nickel, and zinc appeared to
     be inherent in the bottom ash.

 19.  The contaminant concentrations of the disposed ash (i.e., the
     landfill perimeter composites) and the combined ash were not
     significantly different.  This suggests that the concentration
     of the soluble (i.e., leachable) fraction of the contaminants
     compared to the total constituent concentrations is minimal.

20.  The concentrations of PCBs, PCDDs, PCOFs, and BKXs were
     negligible in the field water and laboratory-prepared  leachate
     samples.  Therefore, these compounds appear to be relatively
     immobile in the natural environment.

21.  The QA/QC objectives for sampling and analysis in this study
     were generally achieved.  Although EPA/EMSL is currently
     improving the analytical method for PCBs in ash samples, some
     problems (e.g., low surrogate spike recovery) were encountered
     with these analyses.
                               6-3

-------
22.  All of the data generated in this study was comparable to the
     results from previous studies.

23.  The toxicity Characteristic Leaching Procedure (TCLP) was
     ineffective for extracting the organic constituents including
     PCDOs, PCDFs, and BNAs.
                               6-4

-------
APPENDIX A
REFERENCES

-------
2.0  REVIEW OF PERTINENT LITERATURE
 1.  American  Society of Mechanical Engineera.   Study on 3tata-of-
     t ha-Art, a-f Dioxin From Combuationa Source*.   ASME.  New  York.
     MY, 1981.

 2.  Aaaociata  Committee  on Scientific Criteria for  Environmental
     Quality.    Polvehlorinated  Dibengo-a-dioxina!   Criteria  for
     Thair  Effaerta on Man and Hia Environment.   National  Reaearch
     Council of Canada. No. 18734. Ottawa. 1981.

 3.  Berniaka,  L..  at.  al.   3tate-of-the-Art Report on  Dioxina-
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 4.  Battalia Columbua Laba-Henry.  W.  M.,  R.  L.  Barbour.  R. J.
     Jakobaen.   and   P.   K.   Schumacher.    tnoraanie
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 3.   Behel.  David Jr..  Paul M.  Giordano.  and Don R.  Staphehaon.
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 6.   Burchardt.  X. and G. Baltaen.  Cindera and Reuae.  Daniah Geo-
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 7.   Buaer.  H.  R.. H. P. Boaahardt, and C. Rappe.  "Identification
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 8.   Buttarmore,  William H..  William F.  Lawrence,  and Richard B.
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 9.   Cahiil,  C. A. and L. W. Mewland.  "Comparative Efficianciaa of
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     International  Journal of Environmental  Analytical  Chemiatrv.
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10.   Camp.  Draaaer 6 MeKee.  Generic Environmental  Imoaet Statement
     
-------
11.  Campbell,  W. J. "Metals In The Wastes We Burn?"  Environmental^
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12.  Cavallsro, A., L. Luciani, G. Caronl, I. Rocchi. G. Invernizzi.
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13.  Clamant,  R.  E.  and F.  V. Karasek.  "Distribution of Organic
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14.  Clamant.  R.  E.,  A.  C.  Viau.  and F.  W.  Karsaek.   "Daily
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16.  Concord Scientific Corporation.  National Incinerator Testing &
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20.  Devies,  I.  V., R. M. Harrison. R. Perry, 0. Ratnayaka, and R.
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                                   A-2

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22.  Ouekatt.   E.  J.   "Plant  Saiaaiona-Dioxina  in  Perapective:
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26.  Enginaaring  Scianca.   Suaaarv of MSM Incinerator Aah  Survey.
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27.  EPA.   Dioxin  Analvaia of Philadelphia Northwaat  Ineinaratort
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28.  Fitzgarald.  J.  J.   Statua of Aah Raaidua Evaluation.   OEQE.
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29.  Francia.  C.  W.  Leaching Charaetariatiea of Raaeurea Recovery
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31.  Genetalii,  S. J.. 0. Oorfaan, T. J. Concannon. J. Cirello, and
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     Science & Technology. Vol. 17, No. 4, 1983. pp. 193-198.
                                   A-3

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33.  Greenberg,   **.   &••  <*•  &•  Gordon,  K.  J.  Yost.,  at.  al.
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34.  Greenberg, R. R., W. H. Zoller, and G. E. Gordon.  "Coapoaition
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33.  Haile,  C.  L.,  et.  al.   Aaaeaament of Eaimmiona of Specific
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36.  Hecht,   N.   L.   and  0.  3.  Duvall.   Characterization  and
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     Environaental  Reaearch Center,  Cincinnati,  OH.   Report  No.
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37.  Heimburg,  R. V., A. R. Colella, 0. Jonee, J. M. Rauach, and H.
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38.  Hinchey, H. 0.  Reaeuree ftacoverv and Solid tfaate Hanaqeaent in
     Norvav.  Sweden.  Denmark.  and Geraanv;  Leaaona for New York.
     New   York   State  Le^ialative  Coaaiaaion  on   Solid   Waata
     Manageaent, Albany, NY.  1983.

39.  Jellua,   E.,  A.  X.  Thorarud,  and  F.  W.  Karaaek.   "Two-
     dlaenaioaal   Elactrophoreaia  for  Determining   Toxicity   of
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     1983, pp. 2340-2333.

4O.  Karaaek,   F.   and   A.   Viau.    "Gee   Chroaatographic-Maaa
     Spectroaetric  Analyaia of PCDDa and Organic Coapounda in  High
     Temperature  Fly Aah from Municipal Incineration."  Journal  of
     Chramataqraahv. Vol. 26S, 1943, pp. 79-86.

41.  Kenahan, C. B., P. M. Sullivan, J. A. Ruppert, and S. F. Speno.
                   and  Characteriatiea  of  Munieinal   Incinerator
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42.  Xnudson,  J. C..  Study of Municipal Incinerator Residue and  Ita
     Deaiqnation  aa  a  Danoeroua  Waate.    State  of  Washington,
     Department of Ecology, Solid Waste Section, 1966.
                                   A-4

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43.  Kooke.  R.  H.  H.,  J.  W.  A. Luatanhouwer. «nd 0. Hutzinger.
     "Extraction  Efficiencies of Polychlorinated  Dibenzo-p-dioxin*
     and  Polychlorinated Dibenzofurana fro» Fly  Aah."   Analytical
                Vol. 33, Mo. 3. Narch 1981. pp. 461-463.
44.  Lampsrski, L. L. and T. J. Nestrick.  "Determination of Tatra-.
     Haxa-,   Hepts-,   and  Octachlorodibenzo-p-dioxin  laoaera  in
     Particulate  Samples at Parts per Trillion Levels."  Analytical
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49.  Law,  S.  L.   "Dissolved  Metals  in  Aqueous  Effluents  froa
     Municipal  Incinerators."   Journal  of  the  Water   Pollution
     Control Association.  Vol. 49, No. 12. December 1977. pp. 2433-
     2466.

46.  Law.  S.  L. and G. S. Gordon.  "Sources of Metals in Municipal
     Incinerator  Emissions."   Environmental Science &  Technology.
     Vol. 13. No. 4, April 1979. pp. 432-436.

47.  Lo.   Tssi  Hong.   "Dispossl  of  Municipal  Solid  Wastes  By
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     7, Nos. 2-4. 1964. pp. 73-62.

46.  Lustenhouwer.   J.   W.   A..   K.   Olie.  and  0.  Hutzinger.
     "Chlorinated   Dlbenzo-p-dioxlns   and  Related  Compounds   in
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49.  Mssksrinec,  M. P., C. W. Francis, and J. C. Goyert.  "Mobility
     of   Organic  and  Inorganic  Constituents  from   Energy   and
     Combustion-related   Wastes   Under   Codispossl   Conditions."
     Material Reaeareh Society Svmaeaia Proceedinoa.  Vol. 43, 1969,
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30.  Maynard.  T.  R.   "Incinerator  Residue Dispossl in  Chicago."
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31.  Mike,  J.  S.  and  W.  A.  Feder.   RESCQ Incinerator  Reaidue
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     Recommendations.   Suburban Experiment Station.  University  of
     Massachusetts, 1969.
32.  NU3 Corporation.
     Municipal  Landfill Laaehata  Chagaetariatiea.   U.S.  EPA/OSW,
     Washington O.C.   Contract No.  64-O1-7310, Work Aaaignaant No.
     04, September 1966.
S3.  Ogden  Project*,  Inc.   Reaidue  Saaa^ina and  Analvaia-Harion
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     Marion. Inc.  Report No. 116, December 1966.
                                   A-5

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34.  Qlie, X., P. L. Vermeulen, and 0. Hutzinger.  "Chlorodibenzo-p-
     dloxin* and Chlorodibenzofuran* Are Trace Component* of Fly Aah
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     Netherland*."  Chemoanhare. No. 8. 1977, pp. 433-439.

S3.  Ozvacic, V., G. Wong, H. Toaine, R. E. Clement, and J. Oaborne.
     "Emiaaion   of   Chlorinated   Organic*  from   Two   Municipal
     Incinerator* in Ontario."  Journal of the Air Pollution Control
     Aaaoeiation. Vol. 39, No. 8, 1969. pp. 849-699.

56.  Parker,  F.  G.,  J.  C.  Ouggan,  and T.  M. Cathcart.  Report
     Summary!   Sumner County Solid-Waate Energy Recovery  Facility.
     Vol.  2:   Performance and Environmental Evaluation.  Tennessee
     Valley  Authority and Electric Power Research  Inatitut*.  Palo
     Alto, CA.  1969.

37.  Pohland.  Frederick G.  and Stephen R. Harper.  Critical Review
     and  Summary  of  Laaehata and Gaa Production  from  Landfills.
     U.S. EPA/HWERL:  Cincinnati, OH.  Agreement No. CR8O9997.

38.  Port Authority of NY 6 NJ.   Resource Reeovagy Raaidua;   Rauaa
     and Piappeal.   Engineering Oept., Oe«ign Division*, Office* of
     the  Chief Civil Engineer and Chief Mechanical  Engineer.  Port
     Authority of NY 6 NJ, 1963.

39.  PRC Engineering.   Characterization of Municipal Solid Waata In
     The United State* 196O-2OOO.   U.S.  EPA/OWPE,  Weahington D.C.
     Contract No.  68-01-7037.  Prepared by Franklin Aaaoc. for PRC.
     July 23, 1966.

60.  Rademaker.  A.O.  and J. C. Young.  "Leachata* From Solid Waata
     Recovery  Operation*."  Journal of the Energy  Division.  ASCE,
     May 1981, pp. 17-29.

61.  Rappe,  C.   "Analysis of Polychlorinated Dioxins and  Furans."
     Environmental Science & Taehnolocv.  Vol.  18, No. 3, 1984, pp.
     78A-9OA.

62.  Rappe.  C.  and  H.  R.  Buser.   "Polychlorinated Dioxina  and
     Oibenzofurans in Incinerator Effluents.**  Manuscript, 1981.

63.  Rsppe,   C.,   9.  Merklund,  A.  Bergqvist,  snd  M.  Hsnsson.
     "Polychlorinated  Dibenzo-p-dioxins,  Oibenzofursns.  and Other
     Polynuclear   Aromstics   Formed   During    Incineration    and
     Polychlorinated   Biphenyl  Fires.**   Chlorinated  Dioxins  and
     Dibenzofurans in the Totsl Environment.  Vol.  1, Ann  Arbor, MI:
     Ann Arbor Science Publishers. 1963.

64.  Redford,  0.  P.,  C. L. Haile, and R.  M. Lucas.  "Emissions of
     PCOOs  and PCDFs from Combustions Sources."   The  International
     Symposium   on  Chlorinated  Oioxins  and  Related    Compounds,
     Arlington, VA.  October 23-29,  1981.

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69.  Rghai,   Had!   Oaar.    Phvaieal  and  Chaaiefl^  Bahavior   of
     Chlorinat.ad  Dioxina  on Fly Aah froa  Munieia*^  Ineinarator».
    . Diaaartation, Naw H«xieo Stata University, L«« Crucaa, NM>

66.  Rigo,  H.  G.  Stata-of-tha-Xnowladoa Raoort. on tha Diaeoaal of
     Inelnarator Aah.  Rigo and Rigo Aaaociataa, Duxbury, HA.  1962.

67.  SAXC-Braalatt,  J.,  at.  al.   Coapoaition  of Laaehataa  Froa
     Ae-fcual  Hagardoua  Maata  Sitaa.   U.S.  EPA*  Waahington  O.C.
     Contract. No. 66-03-3113, Work Aaaignaant No. 39-7.

66.  Schoanbargar,  R.  and J. Bandar.  "Analyaia of Matala Found In
     Incinarator  Raaidua."  Proeaadlnoa of tha 1976 National  Waata
     Proeaaaino Ccnfaranea. ASMS. 1976* pp. 499-911.

69.  Schoanbargar. R. J. and A. A. Fungaroli.  "Incinarator-Raaidua-
     FiH  Sita Invaatigation."  Journal of tha Soil  Maehaniea  and
     Foundation* Divlaian. 1971, pp. 1431-1443.

70.  Schoanbargar,  R.  J.  and P.  W.  Purdoa.  "Long Tar» Chaaical
     Laaching  From  Incinarator Raaidua."  Proeaadinaa a-f tha  1976
     National Waata Proeaaaino Con£aranea. ASMS, 1976, pp. 469-497.

71.  Schaub,   W.   H.   and  W.   Taang.    "Dioxin  Formation   in
     Ineinaratora."   EnvlronMantal Seianea fc Taehnoloqv.  Vol.  17,
     No. 12, Dacambar 1982, pp. 721-73O.

72.  Skinnar 6 Sharaan Laboratoriaa.   Taehnieal Raoort. Praoarad For
     Rafuaa  Snarqy  Svatana Coaoanv  (RS3CQ).   Skinnar  6  Sharaan
     Laboratoriaa, Wathaa, HA.  1962.

73.  Surgi,   R.    "Raaiduaa  Froa  Raaourca  Racovary  Facilitiaa:
     Currant  Raaaarch."   Papar praaantad for Signal  Environaantal
     Syataaa at Harina Sciancaa Raaaarch Cantar, Stata Univaraity of
     Naw York, Stony Brook, NY  1966.

74.  Taylor,  0.  R.,  H.  A.  Toapkina,  S. S. Kirton, and D. F. S.
     Natuach.   "Analyaia  of  Fly Aan Producad froa  Coabuation  of
     Rafuaa-Darivad Fual and Coal Hixturaa."  Snvirpnaantal  Seianea
     & Taehnalaqv. Vol. 16, No. 3, 1962, pp. 146-194.

79.  van  dar Sloot,  H.  A.,  0.  Piapara,  and A.  Kok.   Standard
     Laaehina   Jaat   for   Coabuation    Raalduaa.     Studiagroap
     Ontwikkaling   Standaard   Uitloogtaatin   Varbrandingaraaiduan
     (SOSUV), Natharlanda, 1964.

76.  Uaklaoto,  T.  and R.  Tataukawa.   "Polychlorinatad Oibanzo-p-
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     ParaaaetlvM. Vol. 99, 1969, pp. 199-162.


                                    A-7

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77.  Wallinga,  R.  A.  . "That Coapoaition of Raalduaa  from  Municipal
     Rafuaa Ineinaratora."  Environ««nta1 Raaaareh.  Vol.   7,  No.  3.
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78.  Wilaon.  E.  B.  and  0.  J.  Akara.   "Chaaical   and   Phyaical
     Charactarization   of   Hatropolitan  Zncinarator  Rafuaa   and
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     Svaaoaiua. Chicago, IL  197O, pp. 313-326.
                                    A-8

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           APPENDIX B
ANALYTICAL METHODS FOR PCDD/PCDFs

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              ANALYTICAL PMCCDUXC3 TO ASSAY STACX CFFluCKT
                           •
               ANQ RESIDUAL COWUSTIQH PRODUCTS TO*

    OIIO20-P-010XDIS (K90) AND POLYCXIORMATEO OHEHZOFUIUNS (PCOF)




1.  Scop« «nd Applicability of Method


    Tho analytical procedures described hart «rt applicable for the
determination of polychlorlnatad dlbenio-p-dloxlnj (PC90) and dlbenzo-
furam (PCDF) In stick effluents fro» comftustlon processes.  These methods
•rt Also applicable to residual cooftustlon products such as bottom and
predpltator ash.  Tho methods presented entail  addition of fiocaplcally-
laboled Internal standards to all  saapl«s in known quantltlts, extraction
of tfco s«p1t «1tn appropriate organic solvents, pr«llainary fractlonatlon
and cleanup of tht extracts usln? a sequence of liquid cnronatography
eslMns* and analysis of the processed extract  for PCOO and PCOF using
coupled 9*s dirwatoorapny - ous spectrwetry  (GC-MS).  Various
performance criteria are specified herein «nich the analytical data
eust satisfy for quality assurance purposes. These reoresent «ln1imji
criteria Nhlcft oust bo Incorporated Into any proertsi 1n «n1ch K80
and PCOF are dotanrined 1n covaustlon product saaples.


    Tho Mthod presented hero does not yield definitive Information on
the concentration of Individual PC80/PC3F Isoners, except for 2,3,7,1-
TctrachlQrod1b€nzo-p-41ox1n (TOO) and 2,3,7,8-Tetrachlorod1ben2ofuran
(TOP).  Rather, It Is designed to Indicate  the total concentration of
tht Isoaers of several chlorinated classes of K80/PC8F (that Is. total
tatra-, penta*, noxa*, hepta-, and octachlorfnatad 41benxo*p-d1ox1ns and
dlbenxofurans).  Of the 79 separata PCOO and US ?CDF IsoMrs, there
are 22 TCSO, 38 TC8F. 14 PeCOO. 2S PeCOF, 10 MxCOO, 16 HxCOF. 2 HpCOO,
4 HpCOP, 1 OCSO and 1 OC8M


    Tho analytical oothod presented herein  1s Intended to be applicable
for determining PCOO/PCOF present 1n coveustlen products at the ppt to
ppa level, but the sensitivity «*1ch can ultimately be achieved for a
given saaple will depond upon tho types and  concentrations of other chealcal
coosounds In the saaple.
    Tho aethod described here oust bo Implemented by or  under the
supervision of cheerists with experience m handling supertoxlc materials
and analyses should only bo performed 1n rigorously controlled.  Halted
access laboratories.  Tho quantltatlon of PCflO/KDF should bo accomplished
only by analysts experienced 1n utilizing capillary-column gas chreoatograpny.
mass spectroeatry to accomplish quantltatlon of chlorocarbons and  similar
compounds at very lev concentration.
                                  B-l

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        toxlcologlcal data which art available for tht PCOO and PCOF »rt
far from complete.  That Is, tht toxlcologlcal properties of all  of
tfte Isomirs comprising tht 75 posslbit PCOO and US posslbit PCOF art
not prtstntly known.  However, a consldtrablt body of toxlcologlcal
data txlsts for 2,3,7.<-TC80 which 1nd1catas that, 1n certain animal
species, this compound Is lethal at extraordinarily low do«s and  causas
a wldt rangt of systemic afftcts. Including hepatic disorders, carcinoma
«n4 birth defects.  Millt euch Itss data 1s avallabit regarding tht
toxicology of 2.J,7,f-TW. sufficient data 1s avallabit to fora  tht
basis for tht btlltf that 2t3.7,«-TC8r Is similar 1n Its toxlcologlcal
prootrtlts to 2,3,7.f-TC80.  Relatively little Is known about tht toxi-
cology of tht higher chlorinated PC80 and PCSf (that 1s, pent* through
octachlorfnated PCOO/PCOFh although there Is some data to suggest that
certain pent*-, htxa-, and heota* PCM/POJF Isomers are haiardous.  In
v1e« of the extraordinary toxlclty of 2,3,7.8-TCaO and 1n view of tht
exceptional biological activity of this coapound (on the basis of enzyme
Induction assays ) and of compounds having similar nolecular structures,
extensive precautions are required to preclude exposure to personnel
during handling and analysis of materials containing these compounds  and  to
prevent contaertnatlon of the laboratory. Specific safety and handling
procedures which are receamded are given In the Appendix to this protocol.
a.
    The abbreviations which are used to designate  chlorinated d1benzo-p-
    dloxlns and dlbenzofurans throughout this document are as follows:

    PCOO • Any or all of the 7S possible chlorinated d1ben2O«p«d1ox1n Isoners

    POP - Any or all of the 138 possible chlorinated dlbenzofuran Isoners

    TC80 - Any or all of the 22 possible tetrachlorlnatad d1benzo-p-d1ox1n  isest

    TC8F * Any or all of the 13S possible tetrachlorlnatad dlbenzofuran Isemers

    PeCSO - Any or all of the 14 possible pentachlorlnatad d1benzo-p-d1oxln fsor-

    PeCST - Any or all of the 2S possible pentachlorlnatad dlbenzofuran Uomers

    HxCOO • Any or all of tht 10 possible hexachloHnatad d1benzo«p-d1oxln

    HXC8T • Any or all of tht II possible  hexachloHnatad dlbensofuran

    HpCflO - Any or a11 of tht 2 possible heptaehlortnatad d1benzo-p-d1oxln lso«t

    HpOV • Any or all of tht 4 possible neptachloHnated dlbtnzofuran Isomers

    OC80 - Octach1orod1benzo-p-d1ox1n

    OCOP - Octachlorodlbenzofuran

    Specific  Isomers.  -  Any of  the abbreviations cited above aey  be  convtrttd t
    designate a  specific  1 scaur by inoicatmg  the exact positions (carton awr
    where  chlorines  are  located within the nolecule.   For example, 2,3.7,8-««.-a
    refers to only one of  the 22 possible TCOO  Isomers • that Isomer which  U
    chlorinated  In tht 2,3,7,1 positions of  tht d1benza-p-diox1n  ring  structure
                                     B-2

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2.  Reagents


    The following reagents and chemicals art approprfate for ust 1n thtst
proctdurts.  In all casts, tquivaltnt raetrlals from othtr supplitrs
may also be used.


    2.1  Potassium Hydroxide, Anhydrous, Granular Sodium Sulfatt and
Su If uric Add (all Reagent Grade):  J. T. Baktr Chtmlcal Co. or Flshtr
Scientific Co.  The granular sodium sulfate 1s purifltd prior to use
by placing a beaker containing the sodium sulfate 1n a 400 C ovtn for
four hours* then removing the beaker and allowing It to cool In a desiccator.
Store the purified sodium sulfate 1n a bottle equipped with a Teflon-
lined screw cap.


    2.2  Hexane, Methyltne Chloride, Benzene, Hethanol, Toluene,
Isooctanc:  'Distilled 1n Glass* Burdlck and Jackson.


    2.3  Trldecant (Reagent Grade):  Sigma Chemical Co.


    2.4  Basic Alumina (Activity Grade 1, 100 • 200 mtsh):  IO1
Pharmaceuticals.  Immediately prior to use, the alumina 1s activated by
heating for at least 16 hours at 600 C 1n a muffle furnace and thtn
allowed to cool 1n a desiccator for at least 30 minutes prior to use.
Store pre-conditioned alumina 1n a desiccator.


    2.5  $111ca (810-S11 A.100/200 mesh):  Blo-Aad.  The following
procedure 1s recommended for conditioning the B10-S11 A prior to use.
Place an appropriate quantity of Blo-SII A In a 30 ne x 300 m long
glass tube (the silica gel 1s held In place by glass wool plugs) which
1s placed 1n a tube furnace.  The glass tube 1s connected to a pre-
puHfled nitrogen cylinder, through a series of four traps (stainless
steel tubes, 1.0 cm 0.9. x 10 cm long)*:  1) Trap No. 1 - Mixture
comprised of Chromosorb U/AU (60/tO nesh coated with SS Aplezon L),
Graphite (UCP-1-100), Activated Carbon (SO to 200 mesh) in a 7:1.3:1.5
ratio (Chromosorb U/AU, Aolezon L obtained from Supelco. Inc.. Graphite
obtained from Ultracarbon Corporation, 100 flesh, 1-M-USP; Activated
Carbon obtained from Fisher Scientific Co.); 2) Trap No. 2 • Molecular
Steve 13 X (60/10 mesh), Supelco, Inc.;  3) Trap No. 3 - Carbosleve S •
(80/100 mash), obtained from Supelco,  Inc.; 4) The B10-S11 A Is heated
1n the tube for 30 fllnutes at 180*C while purging with  nitrogen  (flow
rate 50-100 ml/minute), and the tube  Is then removed from the furnace
and allowed to cool to room temperature.  Methanol  (175 nt) 1s then
passed through the tube, followed by  175 ml methylene chloride.   The
tube containing the silica 1s then returned to the  furnace, the  nitrogen
purge 1s again established (50-100 ml flow) and the tube  1s heated at
50*C for 10 minutes, then  the temperature  1s gradually  Increased to
iao*C over 25 minutes and  maintained  at 1SO*C  for  90 minutes.   Heating
1s then discontinued but the nitrogen purge  1s continued  until  the  tube


                                  B-3

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 cools to  rooa tewperature.   Finally,  the  silica  is transferred to i clean,
 dry. 9l4SS  bottle- and capped with a Teflon-lined screw cap for storage.


     2.5   Silica Sel  Iieiregnated With  SulfuHc Add:  Concentrated sulfuric
 add (44  9)  1s cotfclned wirn 100 9 8 Jo-Si 1 A (conditions* as described
 afeove) 1n a  screw  capped beetle and agitated to «lx thoroughly.  Aggre-
 gates art dispersed  with a stirring rod until a unlfone •Ixtun 1s obtained.
 TIM  HSOj-sllica g«1 1s stored 1n a scr«*- other suppliers nay
also be used.


    3.1  Glassware used in the analytical procedures (Including the
Soxhlet apparatus and disposable bottles) 1s cleaned by rinsing successively
three t1e»s with nthanol and then three tlavs with Mthylene chloride,
and finally drying 1t in a 100 C oven.  Settles cleaned 1n this Banner
are allowed to cool to roeei tawperature and are then capped using Teflon-
lined 11ds.  Teflon cap liners are rinsed as* just described but are
allowed to air-dry.  Hare rigorous cleaning of sow glassware with
detergent nay be required prior to the solvent rinses, for exaople. the
glassware ea^loyed for Soxhlet extraction of saaples.
                                 B-4

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     3 1.1   Sample  Vessels:   125  (it  and  250  rt.  flint  glass  bottles  fitted
 with screw caps and teflon cap liners, and jlass ttst tubes,  vwR-Sdencific.


     3.1.2   Ttflon  Cap  Liners:  Scientific Specialities Service,  Inc.


     3.1.3   Soxhlet Apparatus:  Extraction apparatus, AlUhn condenser,
 Klmax Brand, American  Scientific Products Cat. No. E52S2-2A.
    3.1.4  Gravity flow Liquid Chromatoeraphlc Columns:  Custom
Fabricated (Details of the columns art provided 1n later sections).


    3.1.5  M1cro-v1als (3.0 at):  Reliance Glass.


    3.2  Capillary Gas Chromatoeraohlc Colons:  Two different columns are
required 1f data on botn 2.3.7,8-TCOO and 2.3,7,8-TCOF, as veil as on
the total PCOO/PC3F by cnloHnatad class, are desired.  The appropriate
columns are:  1)  A fused silica ca1t«R  (40 N x 0.25 m 1.0.) coated
wltii 01-5 (0.2S u f11> tnlcieness), J 4 S Scientific. Inc., Crystal
Lake, II 1s utilized to separate eacn of tne several tetra«throucn
octacAlorinated COOs and COFs, as a froup, frost all of the otner groups.
While this column does not resolve all of the Isomers within each
chlorinated group, 1t effectively resolves uch of the chlorinated
groups frost all of the other chlorinated groups trd therefore provides
data on the total concentration of each grouo (ttut 1s, total tetra-,
penta-, hexa-, hepta* and octa COOs and COFs).  This colum also
resolves 2,3,7,3-TCOO from all of the other 21 TC30 Isocers and this
Isooer can therefore be determined quantitatively if proper calibration
procedures are applied as described further in a later section.  This
column does not completely resolve 2,3,7,I-TC3F from the other TC8F
Isoners, and 1f a peak corresponding in retention time to 2,3,7,8-TCOF
1s observed 1n the analysis using this column, tnen a portion of the
saaple extract nust.be reanalyzed using the second GC column described
below If 1 saner • specific data on 2,3,7,S-TC3F is desired.  2)  A
fused silica column (30 N x 0.29 m 1.0.) coated with OB-US (0.25 u
film thickness), J 4 S Scientific, Inc., Crystal Lake. IL. oust be
utilized to obtain quantitative data on the sancentratlon of 2,3,7,8-
TCOF, since this column adequately resolves 2,3,7,8-TCOF from the other
TCOF 1s<
    3.3  Balance:  Analytical Balance, read1b111ty. 0.0001 g.


    3.4  nitrogen Slowdown Concentration Apparatus:  N-Cvap Analytical
Evaporator Model III, Organematlon Associates Inc.


    3.5  Tube Furnace:  Lindberg Type 59344.
                                   B-5

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4.  Instrumentation

    841 Chromatograph-Hass Spectrometer-Oata System (GC/MS/OS):  The
iMtrumtnt system used ta analyze sample extracts  for PCOO/PCOF
coaoMsts a Sis chroaatograph (fitted for capillary columns)  coupled
dlntctly or through *n enrichment device to a ntss spectrometer which 1s
•oulooed with « computer-based data system.  The  individual components
of tht SC/W/OS art described below.
    4.1  Sas Chromatograph (SC):  Tht Chromatograph out  be  equipped
vfth an appropMatt injector and pn«uMt1c system to  permit  use of the
specified glass or fused silica capillary columns.  It oust  also  Incor-
porate an oven which can be nested In a reproducible, programed
tmmjerariin cycle.  The Injector should be confloured for spMtless/
split Injections.  Tht SC column ptrfoneance should be vertfltd at the
be9lnnln9 of etch 8 hour «orfc ptHod or at the be^lnnln^  of  each  series
of analyses If tart than ont sot of saaples is analyzed durlne, an I
hour shift.  Extracts of coapltx coaoustlon products  and  effluents nay
contain nuntrous organic rtslduts tvtn after application  of  tht axtan-
slvt prtfract1onat1on/c1eanuo procedures specified 1n this eithod.
Thest rtslduts aay result 1n strlous dtvlatlon of SC  coluan  ptrfor-
tance and thtrtfort, frtquent ptrforMnct chtcks  art  desirable.   Using
appropriate calibration Mixtures, as described below, tht retention
t1w windows for each chlorinated class of CSOs/COfs  oust bt vtrlfltd.
In addition, tht SC coluan utilized oust bt dtaonstrated  to  effectlvtly
stparate 2,3,7,3-TCOO fro* all other TOO tsoears If  data on 2,3,7,8-
TC80 alont 1s dtslrtd with at least 201 valley definition between the
2,3,7,3- 1somr and tht other adjacent-tlutlnt, TCOO Isoatrs. Typically*
capillary coluan peek widths (at halfntaxlsut peak height) on tht ordtr
of 3-10 seconds art obtained In tht courst of these analyses.  An
appropriate GC ttaptraturt prograei for tht analysts described htreln
Is discussed 1n a later section (set Table 1).


    4.2  Oas ChroMBtograph-mss Soectroaeter Interface:   Tht GC*MS
Interface can Include anrlchaent devices, such as a glass jet separator
or a s111cont oeeferant separator, or tht gas chroemtograph can bt
directly coupled to tht emss sptctronttar source, 1f  tht  systea  ha'*
adequate punplng of tht source region.  Tht Interface may Include a
dlvtrter valve for shunting tht coluan effluent  and  Isolating  tht
nass spectrometer source.  All coaoontnts of tht interface should be
glass or glass-lined stainless steel.  Tht Interface  components  oust  bt
compatible with temperatures  1n tht ntlghbornood of 2SQ*C, which Is Wt
temperature at which tht  Interface Is typically maintained throughout
analysts for PCM/POT.   Tht  O/W Inttrfact mutt bt approprlattly
configured so that tht separation of 2,3,7.1-TCOO from the ethtr TOO
isomtrs which 1s achieved in  tht gas chromatogrtphlc coluan is not
appreciably dtgrtdtd.  Cold spots and/or actlvt  surfaces  (adsorption
sites)  1n  tht a/W  Inttrfact can caust  peak  tailing and  ptak broadening,
If tht  latttr art obstrvtd, thorough cleaning of tht Injection port.
interface  and connecting  lines should  bt accomplished prior to pro-
ceeding.
                                      B-6

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    4  3  Mass Spactromtar  (MS):  Tha mass  spectrometer  used  for  the
         dascrlbad hara  1s  typically a  double-focusing sactor or
 ua  Instrument aqulppad with an  alactron  iap«ct sourca (70 ev),
•alntalnad  at 2SO*C, and a  standard alactron multiplier  datactor.
If Dosslbla, 1t  Is desirable to hava both lot* and high resolution
capability  with  tha mass spectrometer used, slnca confirmation of
data oOtalnad by low resolution MS using high resolution MS 1s sometimes
desirable.  Alternatively,  a combination of aiss spectrometers can ba
used for this purposa.   Tha static resolution of tha Instrument oust
ba Maintained at a minimum  of 1:500 (with a 101 valley between ad4acant
•asses) 1f  operating In  the low resolution MS mode, and a minimum
resolution  of 1:10,000 1s desirable for operation 1a the high resolution
•ode.  The  mass  spectrometer mat also  be configured for rapid computer-
controlled  selected-Ion  monitoring 1n both high and low resolution
operating Modes.  At a minimum, two lon-evsses characteristic of each
class of chlorinated dloxlns should be  monitored, and these are two
Ions 1n the molecular 1on Isotapic clustar.  It 1s desirable for
Increased confidence In  the data to also aonltor the fragment Ions
arising frooi the loss of COC1 from the  molecular Ion.  In order to accomplish
the requisite rapid Multiple Ion oanltorlng sequence during the t1«e
period defined by a typically capillary chroaatagraphlc peak (the base
of the chromatogrephlc peak Is typically 15-20 seconds 1n wldtb), the
following MS performance parameters are typically required (assuring
a 4-1on Bonltorlng sequence for each class of POJO/PCOr):  dwell  t1m/
Ion-mass, »100 msec.; minimum number of data po1nts/chromatagraph1c
peak, 7 .  The mass scale of the BBSS spec trow tar 1s calibrated using
high boiling perfluorokerosene and/or soae other suitable ness standard
depending upon the requirements of the  GC-MS-OS system utilized.  The
actual procedures utilized  for calibration of the eass scale will be
unique to the particular mass spectrometer being employed.  A 11st of
tha appropriate  Ions to  be  monitored 1n the PCOO/PCOP analyses described
herein 1s presented In a later section  (see Table 1).


    4.4  Data System:  A dedicated computer-based data system, capable
of providing the data described above,  1s employed to control the rapid
selected-Ion monitoring  sequence and to acquire the data.  Both digital
data (peak  areas or peak heights) as well as peak profiles (dlsoUys of
Intensities of Ion-masses monitored as  a function of tine) should be
acquired during  the analyses, and displayed by the data system.  This
raw data (mass chromatagrama) should be provided In the report of tne data.


5.  Calibration  Standards


    A recommended set of calibration standards to be used 1n  the  analysas
described herein Is presented below.  Stock standard solutions of the
various PC90 and PC8F Isomars and mixtures thereof are prepared 1n a
glovebox, using  weighed  quantities of the authentic  Isomers.0  These
stock solutions  are contained In appropriate volumetric  flasks and are
stared tightly stoppered, 1n a refrigerator.  A11quots of the stock
standards are removed for direct use or for subsequent serial dilutions
to prepare  working standards.  These standards must  be checked regularly
(by comparing instrument response factors for them over  a period  of
                                  a-?

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 tlat) to tnsurt that solvent tvapor«tion or othtr  lossts navt not occurrtd
 which Muld iltir tht standard concentration.   The stvtril rtconrntndtd
 standard solutions art as follows.


    j.1  Standard Mixture A:  Prtpart i  stock  solution containing tht
 following Isotopically-labtlltd PCOO  and PCOF  in  isooctant it tht
 1nd1cattd conctntratlons:  2.Sn«./ttluCu-2.3,7,8-TCOO. 2.5ng/u11TCU-
 2.3.7.8-TCOF, ZSntfuL"^-! ,2.3.4,7,8-HxCOO,  25ng/uLlfCia-1 ,2.3.4,7.3-
 HxCOF, 2Sng/uLllCia-OCOO,' and 2Sng/uLllCi»-OCOF. Portions of this
 Isoatr rixturt in addtd to all sacplts  prior  to analysts and strvt
 as Intamal standards for us« 1n quantltatlon.  tacavtry of thtst
 standards 1s also usod to guagt tht ovtrail  tfflcacy of tht analytical
 procodurts.

    S.2  Standard 8:  Prtpart a stock solution  containing 1.0 ng of
 >7CU-2,3,7,a-TCOO/uL of isoectant.  This standard can bt colnjtcttd
 1f dtslrtd, alon? with allquots of  tht final sanplt txtract to rtllaoly
tstlHtt tht rtcovtry of tht uCi»-2.3,7,a-TCBO surrocatt standard.


    5.3  Standard Mlxturt C:  Prtpart a  stock  solution containing
 100 ntVul of Isooctant of tach of tht following PCSO  and POP:
 2.3.7,t-TC8Fj 2,3.7,«-TCOO; 1,3.4,4,|^«COF, 2.3,4,«,7^«CDF; 1,2.4.7.9-
 PtCSO; 1.2.3,8,9-PtC80; 1.2.3.4t«,8.HxCOF;  2.3,4,C,7,i-MxCOF; 1,2.3.4.5.8-
HxCOO, 1,2,3,4,5,7-HxCOO; 1,2,3,4,4,7,3-HoCOf;  1.2.3,4,7J,9-HpCOF;
 1,2.3,4,6,7,8-HpCOO; 1,2,3,4,8,7,9-HpCDO; OCCF: and OCOO.  This 1sow
«1xturt is ustd to dtflnt tht  oas  chronatooraphlc rtttntlon tlat
 Inttrvals or windows for tach of tht ptnta-, htxt-. htpta-, and
octachlorlnattd groups of PCOO  and PCOF.   Each pair of Isootrs of a glvtn
chlorlnattd class which Is llsttd htrt corrtsponcs to tht first and
 last •luting Isootrs of that class  on tht 01-5  capillary SC coluom
 (txctpt for TCOO and TCOF).  In addition, this  Isomtr arixturt 1s ustd
 to. dtttnrint SC-MS rtsponst factors for  rtprtstntatlvt Isomrs of tach
of tht ptnta-, htxa-, ntpta-, and octachlorlnattd  groups of PCOO  and
 PCOF.   Tht lattr data art ustd 1n  quantltatlng tht analytts in unknown
 sanplts.


    5.4  Standard Mlxturt 0:  Prtpart a  stock  solution containing
50 pt/uL of isooctant of tach of tht following TCOO Isomrs:  1.3,6.8-
TCOO; 1.2.3,7-TCOO; 1.2.3.S-TCW; 2.3,7.8-TCOO; and 1,2,8,9-TCOO.  Two of tht
 Isoatrs In this vfxturt art ustd to dtflnt tht gas chronatogrtphlc
 rtttntlon tint window for TCOOs (1,3,8,8-TCOO  1s tht  first «luting TCOO


    b* SOM of tht PCOO/PCOF 1so«r standards  rtcoimndtd for this ttthod
 art avallablt froa Cwdrldgt Isotopt UooraCorlts, CaooHdgt, Massachusttts.
 Othtr PCOO/PCOF standards art avallablt fro* tht 8rthn Laboratory, Urignt
 Statt Unlvtrslty, Oayton, Ohio, fro* tht U.S.  EPA  Standard Ktposltory
 at Rtstarch Trlanglt Part, North Carolina and possibly froa othtr laborttorfts.
 Not all of tht Indicattd  1sotop1ca11y-1abt11td PCOO/PCOF  inttmal standards
 rtcoBMndtd htrt art prtstntly avallablt in quantltits sufficient for
 wldtsprtad distribution,  but thtst art txptcttd to bt availablt in  tht  ntar
 futurt.
                                  B-8

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 Isoaar M* 1,2,3,9-TGO 1s the last tluting TCOO Isoaer on the 08-5
 SC cold")*  Thi remaining Isomn serve to demonstrate that tht 2,3,7,8
 rrgo  Isoaar Is resolved froa Urn other nearest (luting TCOO 1 sowers,
 tnd that the coluan therefore yields quantitative data for the 2 ,3.7,8-
      Isoaar alone.
    8.8  Standard Mixture C:  Prepare a stock solution containing SO pg/O.
of Isooctane of each of the following TC3F Isoaers:   1,3,8,8-TCOF; 2.3,4,8-
TCOFj 2.3,7.8-TCOf, 2,3,4,7-TCDF; and 1,2.8,9-TCOF.   This Isoaar elxture
1s used to define the TCDF gas chroaatographlc retention tlaa window
(1,3,8,8- and 1,2,i,9-TCOf are the first and last elutlng TCOFs on the
08-5 capillary coluan) and to deaonstrata that 2.3,7.8-TCOF 1s uniquely
resolved froa the adjacent-elutlng TCOF iseaers.
8.  Procedures for Addition of Internal Standards and Extraction of Samples


    Both liquid and solid saaples will be obtained for PCOO/PCOT
analyses as a result of the application of an appropriate stack
saapHng procedure.  Saaples
resulting froa the saapllne. train will Include the following (these
will be provided to the analytical laboratory as separate saaples 1n
the fora Indicated):  1) paniculate filter and pertlculatas thereon;
2) particulars froa the cyclone (1f used); 3) ceablned aqueous solutions
froa the laplngers; 4) the Intact XAO-resIn cartridge and the resin
therein; S) coablned aqueous rinse (1f used) solutions froa rinses of
the nozzle, probe, filter holder, cyclone (1f used), laplngers, and
all connecting lines; 8) combined acetone rinse solutions froa rinses
of the nozzle, probe,  filter holder, cyclone (If used), laplngers, and
all connecting lines; 7) coeblned hexane rinse solutions froa rinses
of the nozzle, probe,  filter, cyclone (If used), laplngers, and all
connecting lines.  In addition, saaples of bettoa ash, preclpltator
ash. Incinerator feed mterlals or fuel,  quench liquids, and aitarials
froa effluent control devices Bay also be provided for analyses.


    In general, the voluaes of all liquid saaples received for analyses
are eeasured and recorded, and where appropriate, solid saaples or
allquots thereof are weighed.  Any saaples which are heaogeneous (as
for exaaple, a single liquid phase saaple or a solid which can be
thoroughly mixed) can be split prior to analyses. If desired, provided
that this will still penrit the attainment of the desired detection
Halts for the analytes of Interest.  Saaeles such as particulars from
the saapllng train which are generally collected 1n relatively saall
quantity, are preferably analyzed In total.


    8.1  Organic Liquid Saaples (Acetone and Hexane Solutions)
Concentrate each of the coabined organic liquids (acetone and hexane
solutions) to a volume of about 1-5 a. using the nitrogen blowdown
                                  B-9

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anoaratus (i  stream of dry nltrogan) whilt htatlng  tht  samplt gtntly on a
water bath.   Pool  the concantratad reslduts,  rinsing tht vtsstls thret
tints with small portions of htxant and adding  thtst to tht rtslduts,
and concantrate to naar dryntss.  This rtsldut  will Hktly contain
oartlculatts  which ware rtmovtd 1n tht rinsts of the train probt and
M2z1t.  Comblnt the resldut (along with thret  rinsts of tht final
iarpi« vtsstl)  1n  tht Soxhltt apparatus with tht fllttr and particulars,
and procttd as  dtscribtd undtr Solid Saoplt btlov.


    1.2  Aquteus Liquids
Add an appropriate quantity of tht Isotoplcally-labtltd Internal standard
•Ixturt (SUndird  Mixture A dtscribtd tarlltr)  to tht aqutous liquid
swplt (or an aliquot thtrtof} In a scrtwcapptd bettlt fitted with a
Ttf1on»11ntd  cap.  Add approxlntttly 25X by voluflt of htxant to tht
spited aqutous  saoplt, stal tht bottlt and a^ltete on a snaktr for a
ptrlod of thrtt hours.  Allow tht vtsstl to stand until tht aqutous and
organic laytrs  stparate, thtn transftr tht organic laytr to a stpartte
sa«plt bottlt.  Rtptat tht htxant tatraction stqutitct two additional
tlats and cc«o1nt  tht organic fractions with that fro* tht first ax*
traction.  Procttd with tht saoplt fractionalon and cltanua proctdurts
dtscribtd btlow.


    6.3  Solid  Sanplts
Plact a glass attraction thlmblt and 1 g of silica gtl and a plug of
glass wool Into tht Soxnltt apparatus, chargt tht apparatus with to1 wit
and rtflux for  a ptrlod of ont hour.  Rtoavt tht tolutnt and discard It,
retaining tht silica gtl, or 1f dtslred, reteln a portion of tht tolutnt
to chtck for  background contamination.  For extraction of partlculates,
pi act tht tntlre samp It 1n tht thlrtla ante tht bad of preclaantd silica
gtl (1 cau thick), and top with tht precltantd  glass wool reta1nt<»
froai tht Initial Soxhltt cltanlng prectdure.  A44 tht appropriate
quantity of tht 1sotep1cal1y-!abtlltd Internal  standard mixture
(Standard Mixture  A dtscribtd tarlltr) to tht saoplt 1n tht Soxhltt
thlmolt.  Chargt tht Soxhltt with tolutnt and reflux for a ptrlod of
16 hours.  After txtractlon. allow tht Soxhltt  to cool, rtaovt tht
tolutnt txtract, and transftr 1t ta anothtr saaailt  vassal.  Concantratt
tht txtract to  a voluoa of approxlmauly 40 m\  by using tht nltrogtn
blowdown apparatus dtscribtd aarlltr.  Procatd  with tht sanpla fractlona-
tlon and claanup proctdures dtscribtd btlow.


7.  Proctdurts  for Claanup and Fract1onat1on  of Saoplt  Lctncts


    Tht following  column chroma togrepMc samp It c1 tan-up procadures
are ustd 1n tht orttr  glvtn, although not aVI  may bt  required.   In
gtntrel, tht  silica  and alumina column  proctdures are considered to bt a
minimum requlremtnt.   Accaptablt alternatlvt claanup  procadures may bt
ustd provldtd that thty are damonstrated to afftctlvtly transmit a
                                  B-10

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 representative set of the analytes  of  Interest.  The column  chnwato-
 oraphlc procedures listed here  have been  demonstrated  to be  effective
 fer a trfxture consisting of 1,2,3,4-TCDO. 2.3,7,8-TCOO. 2.3,«,8-TC2«,
 U2.4.8-TCOF. 2.3,7.8-TCOF, 1,2.3,7,8-PeCOO,  1,2.4.7,8-PeCflF,  1.2.3,4,7,3-
 HxCOO, 1,2.4,8,7.9-taCOF, 1,2,3.4,6,7,8-HpCOO, 1,2,3.4.6,8.9-HpCOF,
 OCOO and OC8F

    An extract obtained as described In the foregoing  sections  1s
 concentrated to a voluoe of about 1 eC using  the nitrogen blowdown
 apparatus, and this Is transferred  quantitatively (with rinsings) to
 the combination silica gel coluan described below.
    7.1  Co*1nat1on S111ca Gel Colian:  Pack one end of a glass
coluen (20 at. 0.0. x 230 HI In lenath) vltft glass wool (precleaned)
and add. In sequence, 1 g silica gel, 2 9 base-eod1f1ed silica gel,
1 g silica gel, 4 g ac1d-«od1f1ed sllfca gel. and 1 9 silica gel.
(Silica gel and aadlfled silica gel are prepared as described in the
Reagents sections of this protocol.)  Preeluta the colon with 30 et
hexane and discard the eluate.  Add the saeple extract 1n S et of hexane
to the collar along with two additional S el rinses,  flute the colum
with an additional 90 et of hexane and retain the entire eluate.
Concentrate this solution to a voluoe of about 1 •!.


    7.2  Basic Alumina Coluen:  Cut off a 10 et disposable Pasteur
glass pipette at the 4 et graduation eark and pack the lower section with
glass wool (precleaned ) and 3 g of Woe IB basic aluerlna (prepared as
described 1n the Reagent section of this protocol).  Transfer the
concentrated extract from the constitution silica coluati to the top of
the coluen and a lute tht coluen sequentially with 18 si of hexane,
10 «L of IX nethylene ch1or1de-1n-hexane and 15 H. of SOS eithylepe
ch1or1de-1n-hexane, discarding the first two eluate fractions and
retaining the third eluate fraction.   Concentrate the latter fraction
to about 0.5 oL using tht nitrogen blowdown apparatus described earlier.


    7.3  K-21 Carbon/Cellte 545 Colum:  Take a 9 Inch dlsoosabU
Pasteur pipette and cut off a O.S Inch section froa tne constricted tip.
Insert a filter paper disk at the top of the tube, 2.5 ca. from the
constriction.  Add a sufficient quantity of PX-21 Carbon/Cellte 54S
(Prepared as described 1n the reagent section of this protocol) to the
tube to fora a 2 CB. length of the Carbon-Cell to.  Insert a glass wool
plug.  Preeluta the coluen 1n sequence with 2 eL of SOS benzene-in-«tny1
acetate, 1 eL of SOS eethylene chlorlde-ln-cyclohexane ind 2 at. of hexane.
and discard these eluates.  Load the extract (1n 1 wL of hexane) froa
the aluerina coluen onto the top of the coluan, alone, with 1 as. hexane
rinse.  Cluta the coluan with 2 "L of SOS eathylene ch1or1de«1n-hexane
and 2 et of SOS benzene-In-ethyl acetate and discard these eluates.
Invert the coluen and reverse elute 1t with 4 rt. of toluene, retaining
this eluate.  Concentrate the eluate and transfer  1t to a React 1-ml
for storage.  Store extracts 1n a freezer, shielded fro* light, prior


                                B-ll

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 to  SC-HS analysis.   If desired,  still  another  column chroma tograoMc
 clean-up step can bo employed prior  to concentration of  the  extract,
 as  described below.


     7.4  S1l1ca/01ol Micro Column Cleanup:  After the above  clean-up
 steps  small amounts  of highly colored  polar compounds nay be present In
 complex samples.  These are removed. If necessary, by the following
 column:  Push a smell plug of glass wool Into a disposable 6 me l.d.
 flass  Pasteur pipette, followed by 3 me of Sepralyte (Analytlchem
 International), 6 m of silica gel and finally 3 em of sodium sulfate.
 The column Is pre-wet with hexane, the sample Is applied 1n  100 ui of
 100S hexane and eluted with hexane, collecting 1.5 el.


 8.   Procedure for Analysis of Sample Extracts for PCDO/PCDF  Using Sas
     Cnromatagraphy-mss Spectroaotry (tt-MS).


     8.1  Sample extracts prepared by the procedures described 1n the
 foregoing are analyzed by GC-MS utilizing the following Instrumental
 parameters.  Typically, 1 to 8 uL portions of the extract art Injected
 Into the SC.  Sample extracts art first analyzed using the 08-8 capillary
 SC  column to obtain data on the concentrations of total totra-through
 octa-COOs and COfs, and on 2,3,7,8-TCCO.  If tatra-OJFs are detected
 In  this analysis, then another aliquot of the sample 1s analyzed 1n
 a separate run, using the 08-225 column to obtain data on the concentration
 of  2.3.7,8-TCOF.


    8.2  its Chromatograph


     8.2.1  Injector:  Configured for capillary column, sp11t1ess/sp11t
 Injection (split flow on 60 seconds following Injection), injector
 temperature, 2508C.

    8.2.2  Carrier gas:  Hydrogen, 30 1b head pressure.


    8.2.3 Capillary Column 1:  For total tetra- through octa • CSfls/COFs and
2,3,7,8-TCOO, 60 N x 0.25 me 1.0. fused silica 08-S; temperature  pro-
 grammed (see) Table 1 for temperature program). Capillary Column 2:
for 2.3,7.8-TCD? only, 60 M x 0.25 mi 1.0. fused silica 08-225, twenture
                ; for I «1n..  then Increase from  18Q«C to 2WC t S-C/«m.,
programmed
hold  at 240*C for 1 «1n.)

    8.2.4  Interface Temperature:  2SQ*C


    8.3  Mass Spectrometer


    8.3.1  Ion1zat1on Mode:   Electron  impact  (70 eV)

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     3 3.2   Static  Resolution:   1:600  (10* valley) OP 1:10,000 depending
 uBflfi requirements.   Usually  tht sample "tract* art Initially analyzed
 uslne; low  resolution MS,  then  1f PCOO/PCOf art detected. It Is desirable
 to analyze a  second  portion  of the sample extract using high resolution
 MS.


     a.3.3   Source  Temperature:   250°C


     8.3.4   Ions Man1tared:   Computer-Controlled Selected-Ion Monitoring,
 Set Table  1 for 11st of Ion  masses monitored and time Intarvals during
 which Ions characteristic of each class of C80s and COFs art monitored.


     1.4  Calibration Procedures:


     1.4.1   Calibrating the MS  Miss Seal*:  Ptrfluoro Kerosene, decafluoro-
 triphtnyl  phosphlnt, or any  othtr acc«pttd mass marker compound oust bt
 Introduced 1nta tht  MS, 1n ordtr to calibrate tnt nss scalt through at
 iMit «/x  500.  Tht  procedures specified by tnt mnufacturtr for tnt
 particular MS Instnmnt  ustd  art to bt twloytd for this purpost.  Tht
 nss calibration should bt rtchtcktd at least at I hr. operating intervals.


     1.4.2   Tab!a 1 show  tht tt tonperaturt proorasi typically used to
 resolve each  chlorinated  class  of PCOO and PC9F from the other chlorinated
 classes, and  Indicates the corresponding tint Intervals during which Ions
 Indicative of each chlorinated  class are monitored by the MS.   This
 toaperature program and Ion  eonltorlng t1« cycle must be established by
 each analyst  for tht particular Instrumentation used by Injecting aliquot*
 of  Standard Mixtures C, 0. and  I (See earlier section of this  protocol
 for description of these mixtures)•  It nay bt necessary to adjust the
 taaptrature program and 1on  eonltorlng cycles slightly based on tht
 observations  from analysis of these elxtures.


    8.4.3  Checking 
-------
       of tini Its ptrforaanct can also bo gauged by noting tht peak
        t 1/2 Pt*k ha1«lit) fw 2,3,7,8-TCOO or for 2,3,7,8-TCOF.  If
this peak width 1s observed to broadin .by 201 or tore as  compared to
tht usual width for satisfactory optratlon, than th«  column resolution
1s suspect and aist bt cheeked.  If the colunt rtsolutlon Is found to
b« 1nsuff1c1tnt to resolve 2,3,7,8-TCOO and 2,3.7,8-TCOF  froa thtlr
ntlghborfng TCOO and TC8F Isottrs, respectively, (as  Measured on tat
t»a dlfftrtnt coluars used for resolving these two 1so*trs), then a
    Of-5 and/or Of-225 SC coluen aust b« Installed.
    1.4.4  Calibration of tht «-«-« systea to  accomplish  quantitative
analysis of 2,3,7,8-TCflO and 2,3.7,8-TCOF,  and of tht  total  tatra-
through octa-COOs and C8Fs contained In the saaple extract,Is accoapllshed
by analyzing a sarlts of at Itast tnrtt wsrtlnq calibration  standards.
Caen of thtso standards Is prtpartd ta contain tin saM  concentration
of tacft of tnt stablt-lsotoplcally labtlltd Intarnal standards us«d
htrt (Standard Mlxturt A) but a dlfftrtnt concantratlon  of natlvt
PCOO/PCOF (Standard Nlxturt C).  Typically, «1x tarts will bt prtpartd
so that tht ratio of natlvt PCOO and PCOF to Isotapleallylabtlltd
PCOO and KOf will bt on tht ordtr of 0.1.  Q.S and 1.0 In tht thrtt
working calibration rJxtarts.  Tht actual ctnctntrations of  bath natlvt
and Isotoplcallylabtntd PCOO and POP 1n  tht working calibration
standards will bt stltcttd by tht analyst on tht  basis of tht cancan*
tratlons to bt naasurtd 1n tha actual saopla txtrtcts.  At tha tloa
wnan allquots of tach of tht standards art  Injtcttd (and also whan
1njtct1ng allquots of actual saapla txtracts). 1f daslrtd, an aliquot
of a standard containing typically 1 n? of   HCU-2,3,7,«-TCOO (Standard  8)
can bt drawn Into tha Micro syrlnga containing tnt calibration solution
dtscrlbtd abovt (or tht saapla txtract) and this  Is than co-lnjtctad
along with tht saaolt txtract In ordtr to obtain  data  permitting
calculation of tha parcant rteavary of tht  l*Cu-2,3,7,l-TC50  Intarnal
standard.  Equations for calculating rtlatlvt rtsponst factors fro*  tht
calibration data dtrlvtd frot) tht calibration standard analysts,  and for
calculating tht rtcovtry of tha llCu-2,3,7,S-TCOO and tht othtr
1sotop1ca1lylafitlltd PCOO and POP. and tht conctntratlon of  natlvt
PCOO and PCQF 1n tht saaola (from tha txtract analysis), art  suonariztd
btlow.  In ttitst calculations, as can bo sttn. 2,3.7,8-TCOO  1s tooloytd
as tht 1l1ustrat1vt aedal.  Hovavar. tha calculations for tach of tht
othtr natlvt d1u1na and furtns 1n tht saoplo analyztd art accanpllshtd
In an analgous tannar.  It should bt notad that In view of tha fact
that Staft1t-1sota01ca11y labelled Internal  standards corresponding to
tach tttra- through octachlorfnattd class art not used here (owing
to llarftad availability at this t1a») tha following approach is **oottd:
For quantltatlon of tatrachlorlnatad dlbanzofurans uCi»-2.3,7.B-TCOF
Is usad as tht Intarnal standard.   For quantltatlon of  tatrachloro-
d1btnzo-p-d1ox1w, l>Ci»-2,3.7.«-TCOO 1s usad as  tha  Intarnal  standard.
For quantltatlon of PtCOO, HxCOO, PtCOF, tnd- HxCOP, tht corresponding
stabla-lsotaplcally labtlltd HxCOO  and HxCOF  Internal standards art usad.
For quantltatlon of HpcOQ,  OCOO, and  HpCOP, OCDF, tha 1sotoo1cally
labtlltd OCOO and  OCOF,  respectively, art  usad.   Inherent 1n this
approach 1s tha Assumption  that  tha rtsponst  factors  for each of tht  fsooers
                                 8-14

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flf tach chlorinated class art tht samt,  and  in  tht cast tf  the ptnta-
Imi hcota-COOs and COFs, tht assumption  1s aadt that  tht rtsponsts for
tntst CMO classts art tqulvaltnt to  those for tftt tatra-1somtrs and tht
            , rtsp«ct1vtly.
    8.4.5  Equations for Calculating Rtsoonst Factors, Conctntntion of
2,3,7,5-TCCO In An Unknown Saoplt, and RtcovtHts of Intarnal Standards.
Equation 1:  tasponst Factor (RR5) for natlvt 2,3.7.*-TCOO using
             l'Cia-2,3t7,8-TCDO as an Intarnal standard.
     •htrt:  A,  • SIM rtsponso  for 2,3,7ta-TCM ton at «/x 320 * 322

             A,  • SIM rtspons«  for "Cia-2,3,7,a-TCDO Inttmal standard
              11   1on at a/z  332

             C1s • Conctntntion of the Inttmal standard (pfl./ui.)

             Cf  • Conctntratlon of tht 2.3.7.KTCOO (p«./uL.)
Equation 2:   Rtsponst Factor (W) forITC\ -2,3,7, 8-TCDO, tht co-1njtcttd
             txttrnal standard
             A4c • SIM rtsponst for llCli-2,3,7,8-TCDO Inttmal
              11   standard  1on at «/z  332

             AM • SIM rtspons* for co-lnjtcttd 1TC1,-2.3,7,8-TC30 txttrnal
              n   standard  at «/Z 328 - O.OOf (SIM rtsponst for natlvt
                   2,3,7,«-TCaO at a/z 322)

             C1s • Conctntratlon of tht Inttmal standard (p?./uL.)

             Cts " Conctntntion of tht txttrnal standard (pg./ul.)
                                B-15

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 Equation  3:   Calculation of concentration of native 2.3,7,3-rCflO
              llCii-2,3,7,S-TCDO 41  Intamal standard

 Concentration,  pa../g. • (A,) (I
     where:  Af  • SI* response for 2.3,7,3-TCOO ion it a/z 320 * 322

             Au • SIM response for the llCu-2,3,7,3-TCflO Internal
               19   standard Ion at a/z 332

             I,  • Aaount of Internal standard added to each sample

             M   • Height of soil or «e*te In treat

                 • Relative response factor froa Equation 1
Equation 4:  Calculation of I recovery of "^-2.3.7.3-100 Internal  standard

S Recovery
             A1s • SIM response for "Cia-2,3,7,3-TCDO 1«ternel  standard


             A   • SIM response for ITCU-2,3,7,J-TCBO external  standard
              "   Ion at a/z 321 • 0.009     (SIM Response for  native
                   2,3,7.a-TCDO at a/z 322)

             E.  • Aceunt of "CU-2,3,7.1-TC80 txternal  standard
                   co- Injected with saeale extract (nq.)

             I.  • Theoretical aeaunt of lJCii-2.3,7.J-TCBO Internal
                   standard 1n Injection

                 • Relative response factor froa Equation 2


     As noted above, procedures s1>11ar to these are *pp11ed to  calculate
analytical results for all of the other PC88/PC3F deterorined 1n  this  nethed.


    I.S  Criteria Which GC-m Data Must Satisfy for Identification of
PCOO/PCOr In Staples Analyzed  and Additional Details of Calculation  Procedurts,

    In order to Identify specific PCOO/PCtf 1n satales analyzed, the
      data ootalned must satisfy the following criteria:
    I.S.I  Mass spectril responses aust be observed tt both the Molecular
and fragment 1on Basses correspondlnf to the Ions Indicative of each
chlorinated class of PCOO/PCOF Identified (see Table 1) and Intensities
of these Ions aust aaxlalza essentially slaultaneously (within + 1
second).  In addition, the chroaatoeraphlc retention fines observed for
each PCOO/PC8F slonal aust be correct relative to the appropriate


                                 B-16

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     a~             labelled Internal  standard and oust be consistent
     the retention time winder astablished for the ch1or1n«ted grouo to
which CM particular PCOO/PCOF is. assigned.


    1.5.2  The ratio of the Intensity  of  the molecular 1on (ft)* signal
ta that of the (w»2)+ signal oust be within + 101 of the theoretically
expected ratio (for example, 0.77 In the  case* of TCOO; therefore
the acceptable range for this ratio Is 0.42 to 0.92).


    1.5.3  The Intensities of the 1on  signals aro cons1d«r*d ta be
detectable If oach exceeds tho baseline noiso by a factor of at laast
3:1.  Tnt 1on inttnsitlts aro considered  to bo quantitatively noasurablt
If oacn Ion 1nt«ni1ty excoods tno basoHno noiso by a factor of at
lout 3:lc.


    I.S.4  For rellaala dttactfon and  quantltatlon of FCOT ft 1s also
dtslrafelo ta aonltor signals arising fro* chlorlnatad dlsnonyl othors
«n1div 1f prtsont could give rise ta fraomnt 1ont yielding Ion easses
Identical ta those ean1tared as Indicators of the PCOF.  Accordingly,
1n Taale 1, appropriate chlorinated dlphenyl other aasses are specified
which wst be aanltared simultaneously with the PC8F 1on-«asses.  Only
when the response for the dlphenyl tther  1on eiss Is not detected at
the sam t1oe as the PCS? 1on MSS can the signal obtained for an
apparent PCS? be considered unique.
    I.S.S  Measurement of the concentration of the cangeneri 1n a
chlarinatad class using the eathads described herein Is based on the
assumption that all of the congeners  are  Identical ta the calibration
standards employed in terms of their  respective chemical and separation
properties and 1n terms of their respective gas chromatograpnic and oass
spectrometHc responses.  Using these assumptions, for example, the
"Cti-2,3,7,8-TCSO Internal standard  1s utilized as the Internal
calibration standard for all of the 22 TCOO Isomtrs or congeners.
Furthermore, the concentration of the total TOO present 1n a sample
extract 1s determined by calculating, on  the basis of the standard
procedure outlined above, the concentration of each TCOO Isomer peak
(or peaks for multiple TCOO Isemers.  where these coelute) and these
Individual concentrations are subsequently summed ta obtain the concen-
tration of "total" TCOO.
    c* In practice, the analyst can estimate the baseline noise by Measuring
the extension of the baseline Immediately prior ta  each of the two aass
chromatographlc peaks attributed ta a given PCOO or PCOF.  Spurious signals
nay arise either from electronic noise or from other organic compounds 1n
the extract.  Since 1t may be desirable to evaluate the judgement of the
analyst 1n this respect, copies of original mass chrematograms must be
Included In the report of analytical results.


                                 B-17

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    8.6  Frequently, during the analysis of actual sample extracts.
extraneous compounds which art present  In the  extract (those organic
compounds not completely removed during the dun-up phase of tht analysis)
CM cause chances  1n the liquid and gas chromatographlc elutlon characteristics
of thai PCao/PCOF (typically retention tines for the PCOO/PCDF are prolongtd).
Such extraneous organic compounds, when Introduced into the mass spectro-
meter source My also result In a decrease In the sensitivity of the MS
because of suppression of 1on1at1on. and other affects such as charge
transfer phenomena.  The shifts 1n chromatographlc retention tints are
usually general shifts, that 1s. the relative retention times for the
PCDO/PCOf are not changed, although the entire elutlon time scale 1s
prolonged.  The analyst's Intervention  In the «•« operating sequence
can correct for the lengthened GC retention times which are sometimes
observed due to the presence of extraneous organic* 1n the sample
extract.  For example, using the prograai outlined 1n Table 1. 1f the
retention time observed for 2.3,7.8-TCOO (which normally 1s 19.S el nut as)
1s lengthened by 30 seconds or eon, appropriate adjustments 1n the
programing sequence outlined 1n Table  1 can be made, that Is, tach
selected Ion-monitoring prograai Is delayed by a length of time propor-
tionate to the lengthening of the retention tlavj for the 2.3,7,«-TCDO
Isoaeir.  In the case of 1on1zat1on suppression, this phenomenon 1s
Inherently counteracted by the Internal standard approach.  However.
1f loss of sensitivity due to 1on1zat1on suppression Is severe,
additional clean-up of the sample extract eay be required 1n order to
achieve the desired detection Halts.


9.  Quality Assurance/Quality Control


    9.1  Quality assurance and quality control are ensured by the following
provisions:


    9.1.1 Each sample analyzed Is spiked with stable 1sotop1ca11y labelled
Internal standards, prior to extraction and analysis.  Recoveries
obtained for each of these standards should typically be In the range
from 60-901.  Since these coeoounds are used as tru* Internal standards
however, lower recoveries do not necessarily Invalidate the analytical
results for native rCOO/PCOF, but say result 1n higher detection Halts
then are desired.


    9.1.2  Processing and analysis of at least one method blank sanple
1s accomplished for each set of saaples (a set being defined as 20 sasvjles
or less).


    9.1.3  It 1s desirable to analyze at least one sample spiked with
representative native PCOO/PC8F for each set of 20 or fewer sanples.  The
result of this analysis provides an Indication of the efficacy of the
entire analytical  procedure.  The results of this analysis will be
considered acceptable If the detected concentration of each of the native


                                 B-13

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  PCOO/PCDF addtd to tht sample 1$ within +501 of tht known concentration.
  (An  approprlatt stt of natlvt isomtrs to bt addtd htrt 1s a stt such
  as that Indicated for Standard Mxturt C.)


      9.1.4  At lust ont of the sanplts analyzed out of tich stt (of 20
  samples or less) 1s analyztd In duplicit* and the results of tht duplicate
  analysis art Included 1n tht rtport of data.


     f.l.S  Nrforwnct tvaluatlon saoplts prepare* by  CPA,or other
  laboratories, which contain representative POffl/PCOF In conctntntlons
 approximtinf thest prtsant In typical fltld  sa^lts btlng analyztd
  (but unknown to tht tnalyzln^ lab) should bt  ptrlodlcally dlstrlbuttd
 to laboratorlts aecoopllshlng thtst analysts.


     9.1.6  Sourets of all  calibration and ptrfornanct  standards  ustd 1n tht
 analysts and tht purity of thtst nattrlals sust bt sptclfltd  in  tht dau
 rtport.


10.  Data Rtportlno.


     10.1   Each  rtport of analysts accomplished  uslno tht  protocol
 dtserlbtd  ntrtln will  typically  Includt tablts  of  rtsults which  Includt
 tht  following:


    10.1.1   Ccoplttt  1dtnt1f1cat1on of tht saapl«s anal/ltd  (sampIt
 nuMbtrs and  sourct).


    10.1.2   T)it datts  and  tints  at which all analysts wtr* accasnpHshtd.
 This  Information should  also  appoar on tach oass chronatofram Includtd
 with  tht rtport.


    10.1.3   Raw rnss chromto^raphlc  data which consists of tht absoiutt
 Inttnsltlts  (bastd on  tlthtr  pttJi htlfht or ptak arta) of tht signals
 obstnrttf for tht lonnaissos oonltortd (Stt Tablt 1).
     10.1.4  Tht calculated  ratios of tht 1ntans1t1ts of tht ooltcular
 Ions for all PC90/PCOF dottcttd.


     10.1.S  Tht calculated  concentrations of native 2,3,7,8-TCOQ and
 2,3,7,I-TO3F, and  tht total concentrations of tht congener* of each
 class of PCBO/PCOF for each saaplt analyztd, txprtsstd In nanograos
 TCOO per grast of saoplt  (that  1s, parts-ptr-b11l1on) as determined
 freti tht rt« data.  If no PC80/PCOF art detected, tht notation "Not
 Detected" or •ft.O." 1s ustd, and tht aUnlauei dtttctablt concentrations


                                 B-19

-------
(or dtttctlon limits)  art rtportad.


    10.1.6  Tht sana raw and calculattd  data which art provided for tht
actual saaplts will also bt rtportad  for tht dupllcatt analysts, tht
•tthod blank analysts, tht spUtd samp It analysts and any othtr QA
or ptrfomanct saaplts analyztd in conjunction with tht actual samplt
stt(s).


    10.1.7  Tht rtcevtHts of tht Internal standards 1n ptrctnt.


    10.1.a  Tht rtcovtHts of tht natlvt KOO/PC&F froa splktd sanplts
1n ptrctnt.


    10.1.9  Tht calibration data. Including rtsptnst factors calculated
froa tht thrtt point calibration proctdurt dtscrlbtd tlstwhtrt In this
protocol.  Data showing that thtst factors navt bttn vtrifltd at Itast
ones during tach S hour ptHod of optratlon or with each stpante stt
of saaplts analyztd oust bt Includtd.


    10.1.10  Tht wtlght or quantity of tht original saaplt analyztd.


    10.1.11  Oocuntntatlon of tht sourct of all ?COO/PCCF standards
ustd and avallablt sptclflcations on  purity.


    10.1.12  In addition ta tht tab1«s dtscrlbtd abovt, each rtpert of
analysts will Includt all BBSS chroaatograas obtalntd for all saaplts
analyztd, as wtll as for all calibration, SC coluan ptrforatnct, and
SC "window" definition runs and rtsults  of caluan ptrforaanct chtcis.
    10.1.13  Any dtvlatlons froa tht procadurts dtscrlbtd In this protocal
which art appHtd In tht analysts of saoplts will bt docuatnttd 1n
dttall in tht analytical rtport.


11. Typical Data Ind1cat1vt of Mtthtd Ptrformnct - Prtc1s1on and Accuracy.


    11.1  Tht Mthtd dtscrlbtd htrtln has typically bttn  wploytd ta
quantltatlvtly dtttnrtnt 2,3.7,1-TCOO 1n eotaiiiitlon product sa«Dlts at
conctntratlons as low as 10 p1cograas/gna and as high at 100 u«/g.
Canctntratlons of tht othtr PCOO/PC8T which can bt dtttcttd typically
fall within tht rangt of 20 pIcsgraBf/lsowr/graii of  samplt, ta  100
p1cograns/g of saaplt.  Of count, tht Halts of dtttctlon  which can
bt practically achltvtd art dtptndtnt on tnt quantity of  saaijlt  avallablt
                                 B-20

-------
    tftt atwnt and kind of otfttr 1nttrferr1ng organic rtsldues which art
prtstnt in tftt saaple.  «1tft rtsptct to precision,  tftt avtragt dtv<«t1on
of data ofttaintd from tftt analysts of a nuafetr of aliquot*  of tftt sam
saavlt containing tftt 2.3,7,3-TOO Isontr In tftt 250-300 ppb  rangt
Is tstlntttd to bt +101 or bttttr.  Data on tftt precision of  quantltatlon
of miltlple PC30/PCBF In a ilngle saaplt art not as ytt avallablt. As
v«t, tfttrt Is Inadequate Inttrlabtratory and ptrfomnct evaluation data
available to sotclfy tftt accuracy wftlcft can bt expected of  tftt analytical
procedures dtscHbtd *—*<-
                                  B-21

-------
it *

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        3 II
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               s. s.
   5





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,-sj ssssss
                  .
                  I?


    <* *«
    S3 sa
                 « *
                 a a
              a-22

-------
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                    1

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    ^rttrt.n  |


        i
                s s

-------
        APPENDIX C
ANALYTICAL METHODS FOR PCBs

-------
Netted «M.  OocacBiaMioa at  Moclcidoo  «ad
           la V««o* and Soil/9
    by «»• c&rojM
                          1M3
                    •.
                 VUUJHI U
      9. 1. lavlxaaBMical rroc««clo«
              da«laa«cX» Ohio 4S2<«
                      C-l

-------
 1
 2
 3
 4
 S
 9
10
11
12
13
14
19         Nafa
                 «aa Z4aa«i£ica«iaa
 1         t*i«a»i>ili< «C
 2         KB Caaaaaaxa Oa«4 aa Cilibraaiaa scaoaaxaa
 3         Irtaaa  far fvaaaratiaa af Id Staa* Salaclo*
 4         ?«paaiUua «a4 Appraalmca Caaaanracioaa of Cali&ratiaa  Soiatioa*
           far PttOI-Raafa Oa«a Aeajm«ldaa
 $*        i"i-»p«Lraua «a4 AppraAaava C0a«aa«racioaa a< Calibration  Solaslana
           A* &N Oa«a fcaa^l ittiaa ter Kl Oa«araxaadaa«
 A        Ciapuaicia* aa4 A*prwalaa*a Caa«aa«racioaa ot
           flar SXH Oa«a A«a«lclaa far
                    ter
 7*        Zaaa  tor Salaata* Zaa namiaariaa; ca Oataaiaa KBa  &r
           Oat*  tor raw Sata af <3S Zaaa taam
 7b        Zaaa  tor SalaataA Zaa namiaanjw «a
            ••»«  Zaa Sata af <*9 Zaaa Caa« tor SalMtaA Zaa
                     !taa Oata far KB Zjaaar Qraaaa «a4 Calibratioa Coaaaaara
                tor ialaacaa Zam NaaXtarla* Oar- Aaa^iaitiaa tor »aa«iaida





           Kl Aaalyvaa, Zataraal staaaaraa. tmA Sarraamta Ciaiaanaila
f         T»tiaaUam tor Zatarfaraaaa af KB ruaiiUliif Twa M41tiaaal OUariaaa
14         Carraamiam tor Zatarf araaaa af KB Gamtaiaiav Oma Mattianal Oilartaa
^         *aaa«aar a»4 fvaalaiam af Atttaaataa Haaamramaata af KBa aa4 raatieidac
           la rarvifiai watar
                 laa eorraac praflla of KB caJ4£ratiaa eaaaaaan aad
                    Aaalytaa
           Olaavam laflicatiAv tpprasiaata ralativa rataatloa daaa of KB

                                 C-2

-------
1.  scan AMD
   1.1.   ttU Mttod provido* proeadurM for MM spcctraMcrie aoearainatioa
         otf  polrc&lonaac** blaJMayla (KB*) aad th« U*«*4 panlcidM IA *«
         •oil, or  loittBBM.  Thi* M«te4 tJ apyUeabU to MM*!** eoacalalav
                            or M «aBpl«B •ixcorva, «udi u co*Mr«l«l Aroelon
                                                                         for
                                    e12ltCl«                 309-40-2

                                                             319^4-4
                                                             319-4S-7
                                                            S103-71-4
                                    C19A>C1«                S 103-74-2
                                                           397«5-«0-S
                                                              72-93-4
                                                              30-29-3
                                                              «o-f7- 1
                                                             939-M-O
                                                           33213-43-9
                                                            1031-47-0
                                                              73-20-0
                                    Ct}l«CL«0               7421-93-4
                                                           33494-70-5
                                                            1024-57-J
                                                              73-43-9

                                                           27323-10-0
                                                           23312-42-9
                                                           23323-40-4
                                                           20914-33-4
                                                           29431-29-2
                                                           20401-44-9
                                                           210JS-71-2
                                                           31471-03-0
                                                           33743-07-7
                                                            2031-24-3
                                    C-3

-------
   1.2  Oacaoxioa Ualta vary 4aaa* aacaod aaalytaa »ad vita  aaayla aacrix,  saapla
              atloa procadoraa* condition of caa GC/W rrataa* cypa of  data
                   u «ad iadividoal aaarplaa.  taa cilmUtad  aaeted data«*ioa
        Uait (MR.) far aaea paaticida ia farelflad raaoaac vatar  oxcraeta aaalTxad
        vita full-raaoa data aeajoiaitiea la praaaotad la 3a«t. 14.   Aaalyaia of
        oaU&ratioa aalaxiaaa ^adioatad caat tlh^t oalcnlatad (B^a *1ir aot accarataly
        faflaat iaatxtawatal dataajtioa Ua&ta*  ^ha folloviav vvidaaca  la baaad oa
                           at eallBra«iom aalotioaa vita oaa iaatraaat  ovar  4 pariod



        aaaft.  Wita aalaetad lea aaajtariaa (3X8) data aafataitiam* paa«ieida
        aaalyta datacaioa Uaita 4ra lovarod by a« laaat a factor  of flra.  Oataetiaa

                     \, vita caa dataotioa, Uao,« far liaitadilarnaipaaayl baia«
              $•10 tia*a ^*T^*^T caaa caat. of a aaroxrhl umblithaiiyl •   K aoaocteloro"

                           itaiaa 1 a« 4&d C«U-raaja« data ara
                  LLait far total 9da vill dapaad oa caa
                           ia*.  sat data 4*ajaiaiti0a pracaavraa cadoca  caa datactioa
        Uait far fda by at laaa« a faotar of earaa.
2.
   A 1-t ««car aaapla ia aiaaaA ia a aaparatary ffoamal 4aa*  awcraccad wt«n •a«aylaaa
   calarida*  &epra*«ia«a aitraeviaa araoadaraa far  aail/aatfiaaoc saa*)JLaa will ba
   •44*4 «a«a ravalsa *r« ntnri1na< froB aaaalaf aapariaaa«a. tlia  axcaraes la dA»d
   4a4 aacaiaaail ea baaaaa avria* eoaeaasra«lea «a 4 fiaal  waluaH) at 1  ad ar laaa.
   Saopla «rtra«« «aaaa«aa«a ara aaaarsvaA vita aaaiHary «altaa>  ama caraamcaaraptty
   (QC) 4a4 14aafi£iaA aaa> aaaaiaraA vita lav raaalot-lM*  alaavraa laaji^atiav aaaa
   •paauiaam-j (W).  Aa latatCaaaA data «r*«aa  (09) ea  aaatral  data 4eqoi«iciea
   aad ca saara* ravriava, 4ad aaalpalata aaaa taa«tral data ia aaaa*cial.  Cis&ar
   full-«aa«a ar »alaa«aa>»iaa aaalcartnf (SXll) data  4ra ii»pai'ad, dapaaiii
   eaaaaatraviaa raaaai af eaaaan*  X£ ffaU-raaav data ara  aaipilrad, 4ll
   aaalr««« caa ba IdaatXfiad aa* aa«a«rad vita OM  Oe/M 4aalr*i**   — «11 p«a«X-
   eidaa 4a4 fda aavt ba datasalaaA *a4 if sat data «ra
   da«ae«iaa Uai«a* ev« QC/W 4aalr««* 4ra aacaaaary, aaa  ca  dacaat aad aaaavra
                                                                         a«aadarda«
                                                                        bafara QC/W
                                                                  ia«.  All paa«icidaa
                 • raapaaaa of aaaa «avpaam>4 w tte W laapaaaa of caa iatanal
            vita 4C raiaaiHa tla« aaarar that of  tte paatiaida 4««lyta.  T&a
           I aaaa)la oaajtaaAaatiaa vita taaasiaal oalardaaa la ladiaatad by Idaat^i*
   fl«atlaa aad aaaaaraaaat of cte tw« aaat panirtaax oja»aaanta» jaaaia-rtilardana
   «ad naaaealar.  (Xlpaa-«alardaaa aa4  Boptaaalar< otter aajor caaeoaaa«a of
   caoftaieal Alordaaa* aay 4laa ba praaaax 4ad vill ba
        caia aataad.)
   •da ara UaatXflad 4ad aaaatarad  aa  laaawr froaya (!.«., by la^al of chlarioaeion).
   & ceaaaacxatiaai ia aaaa«ra« far aaaa fd tauaair 9*0091 total Pd ooaeaacration
   la aaoa aaaipla axtraot la obtaiaad by maaUat iaaawr aroap ooacaatrationa.

                                      C-4

-------
                         ira aro oaod aa calibration fftaadarda. aad oao iatoraal
 •taadard,  cftryaoao"*^,  la oaod to eaUarata M roapoaao ee VCBa, vUaoa aaaplo
     Ltloa* rorolro  tao oao at tao aocoad iataraal •taadard, phonanthraao-di a.
 3.1  coneamaaxcm catmuno aotarzev (cat) — A aaia*iaa of aotao* aaaiytao
           ta oaJOferaca tao MM •powi-naaior roapoaaa.
 3.2  O3WUU Maon — T&Tna^teoat. cftia aatted* latflTtdaal KM* «r« da«erlb«d
              Miafcar «Mi9i«« br »«U««tal«w aaA S«li (2).  (thl* auabtf t»
               to da«orib« ffO eaa««a«n la eataloyt yvotemd &y Oltra Sciantiiic,
         I, XT.)
 3.3  CfSZNUU. TPMPMC — A p«r« manual add«d «a « Mupla «RTMC ta taown
                                                                 oehar eaapeuada
                                                             b« «
3.4  UMUSQKT OOfUSJ&tt (101 aad\ LS2) •*^*a saMBvla aLl^oava *ih^n la
                                        vie* lrta««i«aA jgoaaAuraa.
                   daaltca«aa Ia41ea«aa gradalaa iaaa«l«tad vita laboratory
                                                             or rtara^w srocodacaa.
3.3  UJOXA7QXT 7SXTOMMKZ OXOC SOL07XOM (UC) — * aoltzftioa of avehed aaalr«M,
     •utiu^ca eoapoiiaiia, aad lacanal naadaxda oaod ta rrmluata ta« pcr^oraaae*
     of tto 
-------
   3.10 mammae* trnxaaza* SM9U — A aaaal* coairatnln? IOMWI eaaeaatratloaa
        of aa«a»d aaalre** taac haa b««a aaalyxad *f auleipia Ul»ora«erlaa to
        teeaaddM reattaticaily taa aceancy aad praeiaioa that eaa ba «xpac«ad
        vnaa « aaeaed la 9«x«oxMd br * ccapacaa* aaalyat.  Aaalr*« eoaca0«raciona
                    eo taa
   3.11 QOXtrrr conraot (QC)

        aC taa QC
        taa aaalyaia la


                 ta a aaa»la aliqaat bacora artsaetAaa aad la aaaaorad wtca taa
                    raa uad ta aaaaoca •«•»!• eaaaaaaata.  Aaaactatad wlta
              ita caaaaaad *ra twa valaaa* laaarmcary aarraaata
              (UD aad latooratarr awroaata aalka • taaavatxeai
                    tt a aorraaata eaaaaaad la oa aaaltar aatnad parfai
                    aaia.
4.
     sSS.
   4.1  Xa«acfar«aaa« aay ba OMaa4 by eaac«Blaaaca ia wlv«a«a.
        aad oc&ar aaapia pro««Mla« a^aXaaaac*  Labacacary raaaww blaaJca  (UBa)
        a«a aaalysa* ravciaaly ta daaaiM«rae« tiia« taaaa aacarlala ar« Sr«a o<
        lataxfavaaeaa waar taa aaalytloa^ eaadlelaaa «aa4 few
   4.3  90 alalaKa lacartaraaaaa* flaaavara (Ualaalaf aaaaia baetlaa)
        ba aaxXcBloaalr claaaa*.  JU aaaa aa aaaalAla af«ar oaa, rlaaa fUa«var«
        «1«A cfta laa« aal^aa« «aaa»  tSiam «aaa «l«ft aaM»aaa» la hat xatar aaa
        riaaa «tta taa «a«a* «aUawa« by 
-------
                                                  -01 —
      »T »•*» «*T»«P




   *9&O9A0ftl
*»oi m DO*
   9»-OOC — HMT4
             ••WTi >•••! V»^»
fft
                               »*ft
mrr* ••
 •w nsrn »T«
              W*» OS • «l X
                                                                t*r*»
                                      "3-t —
                                                                r*t*t
                         rr
xo i-i (ff
                                                            on
 V  *pecR( *
                                                   "7
                                                                      1*5

-------
4.3  (JOHWMJttZSD (SC/MB STTTJEM
    4.3.t  tno «C mre bo capaalo of toaporaeoro prooraaBiaa aad bo
           wica All roajoirod accaaaoriaa, such aa •yriaoaa. oaaaa, aad «
           colua*.  Tao QC iajoeeioa pore aaatt bo oaaioaod for capillary eoluana.
           Kaaaal tplitlaaa iajocelaaa war* oaod to aeajoir* daea uaod aa cao baai«
           Cor ojaality eostrol roo^lxoaoaca.  Aa aacoaa«ie lajoceor, oevovor, la
                              it •haald pvovtda lor* praoLM r««aaclea «!••• &ad
               alnlatta* wtca tau r«rti«t«n«.  vt«a MB
                             of tlM lav t«ift«l HBTiiaa taavaracara r«^oir«d for
                                will caoa« 1rr^prneaa ra««
                                                                      or fi-r*
                       far «*«a a«aXtar«4 toa walla « saapla «a«faa«a« «lue««
           from tte «C«  TSio M mart prodam * a«aa rpaccroa a*««la* til cris«ri»
           for <20 af of aMafluerovrlaaoarlplMavalaa (OfTT*) iavroaoaod titrauo*
               QC
                                 BOB (OS) i4 roajolrod ca acajolro, rcaro,
                           spoocral dmca.  taa Of amre bo capaalo of
           a daca fllo far rpao^fla iaaa aad placdav iaa aooAdaaaoa
           or •paocna rniahor ca pradwra «olo«tod ioa otrroa« profllao (StCT«)
           aad oauautad ioa carroa* profilao (XXCM).  AUa roa^irod i« cao

                 or •paouoa aoaa«ra la StOa or CXOa.  tcmal dmea aeo^ijizioa
   4.3.4   CK Op«iaa — for S&t daca aaa^iAitiaa. caa Of aaa« bo o««i9pod
                    oapaalo of aea^iriaa; da«a for anl&ipla oroopa of iaaa.
                   • ama« allow a««aam«ad aad rapid caaaooa of cao soc of iona
                   iltavod*  To aoa^lro all m daca aaodad far taploaoncauion
                         Lf-iTaUaala avcaataaad ia«arpro«a«ioa proaoduroo. caa
                                                    daca far fear oraapa  (or
                      i> oaaa ooaalaciaa? of jt)>9 iaaa or far fiva fvaapa of  <,20
                   k«  flM c^Aaa apaa>c aaalcarlaor iaaa dodao^ aaaipla aaalyooa
                                                   eallaraciam aalacioaa  war*
4.4  OC OStOMI —  * 30 a X 8.32 mm SB fmaaA sllloa capillary aoloam eoavaa
     a 0.25 « or thlokar tUrn croaaUafcod paaayl aacttyl ailiaoao  daca  aa
     Dttrapoaa-i (D»-«), J aaa W Scloaelfia, lUacfta Cordova. A) or polyaiphoayl.
     riayl diavcayl silMaua (sacft aa «-«4, Ulto«h Aaao«ia«oa, Ooorfiold.  ri)
     i« ro^xiroa.  Oporaciav caaaltieaa loioim ca prodaeo aoeop«atolo r««ulsj  WXCA
     caoM coloaaa ar* *hawm La Taalo 1? •opara«iaa of pooxieida aaaly«oa  aad 9C1
     eallaraciaa canovaon wica a OB*9 eolujai aad eaooo oporacia^  condieiona i*
     shown ia Fivoxo 1.  to«oa«ioa tiaao na*o boon r«pore*4  (4) for all  20*  PCI
                                    C-8

-------
                                       6-0

                                                          • I
                                                            »*•*•*
                                                                          i'i
                                                     •*9 Ana  ••pnp**»t
                             01
    tea «•<»• p*8TT*oot7*» • VST* •T%**9 ««q*t n V?
                                       « ooi
                   ye A tt't •**»»TO —
        ?»
                                                   tw ntnotiicp am


   •» 1000*0


   i»»a 90

                * •*
aej

-------
7<9  VCB RXSBTIUB JIJJ1E (JUNUMKM fOK SZM OATX  Afc^vi 13 A SIOT QPTXCtt — Kaevlad
     of taa rataa«loa tiaaa of cartala conoaaara  la  nairaaaary  to dataraiaa
     vaaa eo aea^lra data wita «aatt  ion  avt*  TMO caaeaatration callbratloa
     eoaoaaara alao aarv* aa rataacxo* tlaw caaqaaarat  taa 8ir*t alutia?
     d1-»Cl ttrltrt*** taa tla* wfcaa data aeajolaltloa aoax ha»« ba«a
     for loa M« H, aad tta dto-Kl iaalcata* «da« all »da  acv« alu«*4.
                                    oea«*  to*  M«a  (S«c«.  9.4)

7.10
    7.10.1  y«a«lelda Stack Solocioaa —   rrapam  £ro« ptva rcaadard aa«aviala.
                  apyroxlamtaiy 25.0 a* (wt«h  «eeora«y of  0.1  *f)  of cacti
                  tea empauad aarf «a«& pura paa«l«lda aaaly«a«  axeaae
                   Caa X aa4 Kadoa«l£aa XX.  for thoao swa paveleidaa* arapara
            a no«k aala&laa e»lc« aa ceae«a«ra«a4 aa  s&ac prapaxad Jar ocitar
            potftXelda aaaly«aa.  Oijavlw  aaaft uuapaiiaJ la Itaaaa*  aatf dlloea ta
            wlam la a 10-«L (S-aC. for t&a am rtHnatilfitia) valumule 21aak.
            (Caaoaacra«loa at aaaH aavavnaat • 2.3 aa/ab.  asaapc Xndoaol^aaa,
            vkiaH ateold ba S aa/aC.)   Saallav «r  larfar valuava a( reoek
            aay »a oaa4 ti aaaicoA.  If «ava««B4 pwltr la «arei£la4 a
            caa welaat saa ba oaa* wteft*«« garrooloa  «a ealeulaca sfta concan-
                       caa ««ock «eaaaju4  aola«la«. CaaBareiallr  praparad
                            la ha«aaa eaa  ba aaad  at aay caaeaaezaclan li s
            ara traeaaala ta Q9OA-«appl^«d «taad«rda.
    7.10.2  Paatlaida Pria«rr Otlotlea Salocloaa  — I eaoranlaas apprc
            •alotaoa praparatlaa la  to prapaxa tMa paatleida priawry diloclaa
            aaloclaaa taat ara  onaa taa aanaaaayatlaa a< tha 41«*aa< eoaeaatrat^aa
            callaratloa  aalocXam raa^lrad.   taaaa aalocloaa aaa tftaa ba dilixead
                            praaara  all aaadad oallbratloa aaUtclatta.  Ona aa
                            alaaayda aad oaa «a«a aa«« bacaaaa t&a aadi
            calxbratlam  avlatloa doa« a«t oaatAia aadrla aldaayda.  ?Uca 1 at.
            of aaaa paatialda aaalyta/swraawta aaataoqad «ta«ft aelatlaa la *
            23-«C.  laliiaarrln flaak.   (?a«al «alaaw ear all 22 paatielda aaalyvaa
            aad 2  aminaata mamuuaaa • 24 ad.) iUka ta ivloa* «ltft baxaaa aad
                wall*  (CoMamxacla* of aidaanlfaa »afa«a» aodaamlfaa X aad
                       XX • 200 H"t/iii tmfitwt^^1 
-------
                                       vita taa taallaat paaaiala «o
            haartapaca» and loaning vlala ahoold b« -itn1alT«i1.

    7.11.2  KB Prlaary Dilation Standard —  Taka aU*aa«a o* taa scoc*
            •alacloaa of taa aiaa KB oaaeaatratioa calibraeioa cea«aaara tad
            mi* tnfathar ia taa proparcloaa of oaa part of aaea aalatioa of tha
            d, (»1), Gj («), 4»d C13 (»») nanaaaan, CM pare* of aaeH aolutAc
            of taa a4 (MO), 0* (M7), aad O« (»1S4) eaa^aaan. tteaa parta
            a« aaaft •loftlav-oC tte a? (*1M) and Oa (*200)  oaa^aaara, aad fi-rt
                     taa dig (»20») Baatiaar aalatla*.  (Vocat  Tha rwtaatloa
                           daaaritowl la Sa«c. 7.9 aca aoj laaXadad ia tha KB
                                        •aaaa ttttay «ra aoc n«dad for fail-ran?*
            data aa^alaieiam.) TlUa will prvrlda a prlaaxr dilatXaa •caadard
            wlocioa «< taa anapaaAUoa sbawa la TaAla 3.  CaleoLata t&a eoaeaa-
            tcaciom ia ««/uL« «aa tftraa •i9atffiaaa« Clfvaa.  FUea aaeft tolation
            ia a alaaa fiaaa vtal with a ?aflo*-Ila«a acrav eay aad rtara at
            4«C.  Mask taa aaaiama «a taa rial wall t» aaaitar aalmiaa
            dvlav •vca^ar wloclaaa ara natola InaaftnUtaly l£ Mlrvat cra
            ratiaa ia prvwatad.
                                       w (Ctta).
     7.12.1  a aalotion »1 (far fuli-raa«a QX*1  — «aiaa 7.S  ay • 0.1  a*
                -  -  •      •      •     -  ayyioaa-dt2»  dlaaalva  ia haxaaa and
                      i 10 aL ia a *»lnaa».rle flua.  (Coaaaatratloa of
                  750
7.12.2  a Mloaiaa »2 (far SZM OkU)  — Taka 1  tf. at  3  Mlnclaa »1  «ad
        dllsaa u 10 ib ia a wlaaavrla flaak.  (Caataatyatlaa «t «aca
        a • 73 a*/*b>

                                                      wlotiaaa ara

                                                    iadiTidval
                                                                            da
7.13  CU4 POlt FQUHUKI QaXJl
            aa. taa aiaa K| aallkra
                      aad
                     v»a ia Taala 4.)
                   aa, ba«a •
                           aa ia CMC*
                      taa« allow ia)a««iaaa a<
                   evvrlaadiaf
                                                                   i.)
                                                  (Hl«h OIL)  ara praaaa« «e
                                                       wltbavt n saturation
      7.13.1   Tha. r«U*Kaafa m«a Ctt eaa ba prayarad bf aftxlaa1 «^aal pertlona
              o<  taa KB prlaary dllatlaa Mlotla* aa4 tto paaxleida prlaarr
              dtlatlaa Mlualoa taa« coatalaa vadsla aldakqrd* aad than addia* *a
              •pproprlata f«luaa *t a salociaa *i. For inaafli,  1 at. of «aea


                                   C-ll

-------
                 priaarr dUatlaa •oloeloa aad 20  oC, oC  Si  Mlaeiaa «1  proved*  «h«
                 •aproariata caaeaaearacloa Cor Kloa CM..
         7.13.2  Oe&ar full-raafa  OtU  ara pr*par«d by dllueiaw; eha priaary «ilu«Aoa
                 reaadard joiatiaaa  aad addtaa; efca  aapropriaea  aaauae of  IS M
                 • 1.   OUKXOHt   «w  paaeiclda prlaacT dHatioa  standard that,  ra«aa«4,aa elaa oaaoaaari.
         eba« ara taaad ea oataJiUali rrandieiaaa tor SIM data
   7. ij  rr«aar« a wloelaa of twrajata a»fi»ai1t la a «a«ar alacidl*
         m fvovtaa a eaaaaavaciaa la eba aaaaia/blaak ««cra«c «ha« U aaar
                   tr»tlnn aa«l«laaead far aaalr*** **«*« *• *!!**•* «f >20 o& La
               ca taa aaavla ba

   t.l  WOOL UKVUB
        1.1.1  saapiaa aoac ba «allacBad la claaa (««««. 4.2) flaaa caacalaara.
               •aaat  «aa laapln aca aaclalaaaad ca caacala law caa«aacxa«loaa
               ttf aaihad aaaiftaa* a aaapla lar^ar cbaa i-t aay ba naadad.  Aa

                          yvaa la ca add a parvlaa a( anraavlav aal««a< ea

                             am ayf*oarla«a atl^ta* «*iua» U ayamaAaauaiT  1
-------
      0.1.3   SaaaUaa  sheuld ba octractad withla 7 daya aftar eolla«tioa aad aaalyvad
             wltala 40  daya altar extraction.

 0.2   SOIL/SID OUST SM7LXS  —  Approprlata pracaduraa will ba spacifiad whaa
      raavlta ara oataiaad froa aa^elaf
Oaa»aatratlaa aad  daaaamtatiaa  ot  aaaaptaala j til rial  calibration la raojwLrad
baxara aay laaplaa ara aaalytad  aad la  raajolrad  lataraittaatly threaonaut
aaayla aaalyaaa aa dioeatad by raaulta  ot  eaaclavlaa; caXLbratloa diaeka.

      t» raajoirad  at tha baqiaala*  aad  aad ot aach I2«a pariad dariav whieh
         ara partamad.  ma Naditaa CUa far  paaeloida datasaiaatiaaa da net
               aldahyda.  tola allawa tha  Itadloa GO. ta ba oaad far
               «ka, Ualadtaa; a  chaeft ta •aatara  that aadria ijaouapui
            . taitial eallbratiaa a laaarata  Nadloa OS. eoatalalaa '	
         aad tha lataraal ataadard  la aaalyaad ta dataxatfjM tha raaoaaaa factor
(a* aadxia Udaiqrda.  f!iaraa» aalatlaa and
                    a aaaa aaaaama taa« iaaladaa  data  far  a/a  43-430.   u tha
                               Mt all aritaria  (Taala  •),  tha  « aaat  ba
                               •M< all aritaria  ba£ara  prmraadiaa' with
     9.2.3  FiUHIaaaa CaUteatlaa — Za)a«t a  t- or  2-«t itlip«^ ot taa iiadlaa
            CK aad aaajpira data fxaa a/s 4J ta 910.   AaajHra >9  spactra doriaa;
            	^   gi «C aaaa.  Tatal «yala tlaa aaamld ba  >0.9 a aad fl.S •
                ^1.S a.                                                  *
            CMTTXOMt  Miaa aaa^iriaf SZN data. «C aaaratia^ eonUelaaa aoat ba
            earatfolly rapredaaad tot «a«h aaalyaia  ta prortda raoredoeidla
            r«taa«laa tlawar Lt not, iaaa will aot  ba aeaXtarad at uia


                                    C-13

-------
    9.2.4.1  sat Calioratioa for TCJ) daearaiaatioaa

         9.2.4.1.1  TV« optlaaa far 3ZM data acejoiaitiaa ara provided.
                    Data caa ba acquired vita four *ata of  f K> aaaoaaar *104, taa firrt
                             Stay aaajviaitiaa vith Zaa tot »2 aad bo^ia
                            Laa vith Zaa tot »3 Jnat (approxlaatalr  10  •)
                            ttiaa of TCI
                      _
                    C14-TC>.  Stay ao^alaieiaa wiea Zaa S«« *3 aad  aayla
                                       a fl«« M )vae ( aasroi^aa«aly 10  i)
                                        , 2-4,4'-OOT.
         9.2.4.1.4  9ai d»«a iB^tUltiaa with tivt laa s««a.
                    omta wtta OM fawr Zaa S«ca 4aaarlb«d la s««s.
                    9.2.4.1.3 aad add a flfcH taa S«« b^iaala* data
                                 lsa «aa« M« )ua« ( lafcnwl M«iy  10
                           •Imlaa «* TCI eeaaaaar *20«, U* iirre
                            CL^
9.2.4.2  SZH Caliaratiaa tar 7«a«ieiao 0««axBiaa«iaaa — Tir««
         ^19 iaaa aaeJi ar« oaod (Taalaa 9*10).  t«tla data
              Zaa tot »i bafar* «iation of alaaa-nc. tJu

                 of aldria aad bafam alotiaa of haptaaftlar oaoada.
              aa^aiaitiaa vith Zaa tot *2 aad Turin aeajaiaitiaa vith  Zaa
             •3 afta* aiatiaa of aadaavlfaa ZZ aad bafara 4,4'«OOO.
9.2.5.1  r«U-«aaaa Oa«a
                             Aaaiyaia of Nadloa OU,
        9.2.S.1.1  «C paifaiaiaaa — aaaaUaa ••aaradaa of b««a-MC
                   aad •maawOC; baaaliaa •aparaclaa of aadrla kacana
                   aad c*arr««»«"»i2t  Baiaft« of ClfTCB paak ^«0%  s«ca«9MC
                   paak hoioBCt  hoiaa* of earyaaao-d^ P*** i*0%  °< ^*
                   paak haiob* of aacaaxrealar, walea aay  partially co«lus«
                        taa ClfKS
        9.2.3.1.2  HI aanaitlrtcy — Siomal/aaiaa  ratio  of  >9  far
                   a/* 499 of KB eoao^aor  »209, C110-K3).  *
                          C-14

-------
                   M calibration —  Aboadaaca of £40% aad <60% of
                   a/s S02 ralatlra to a/s 499 tot tea conMnar »209.
        9.2.5.1.4  Lack of 4o«radatloa of aadria.  "••-Ini aa axtractad
                   loa earraat profUa (KCT) Cor a/s i7 la too rataatloa
                               boewaaa 4,4'-OO* aad aadaaulfaa solfatof
                           taat taa aboadaaea of a/i €7 a« tha rataatloa
                           aadrla aldaayda la <10% of taa tttMn-ian-t of
                   a/i «7 groiaurt br •adxla.
        9.2.5.1.5  Lack of dacracaftLaa of 13C12-4,4'-OOT.  teaalaa t!C?«
                       a/s 25* aad a/s 247 la taa rmaa«ioa Uaa window
                   eaat lacladaa 4,4'-OCO, 4.4'«OOC aaa 4,4'-oot> a/s
                   2St woald ba pvocoeaa by 13C12-4,4'00«, aad a/s 247 by
                     C12-4,4'-OOO.  Caaflza tha« taa totai aboadaaca of
                   boca laaa U ,S for a/s
                    49» of KB oanvaaar «209, d19-»d,  aad Tor a/s 241
         9.2.5.2.3  MS calibration — Xbondanca of £79% aad <99« of a/s
                    500 raUtiTa ea a/s 490 far coa^anar »209,  Ci1Q-fC3.

9.2.5.3  SSI feasiciat Data

         9.2.5*3.1  OC •oyantioa —  iaaallaa saaaratloa of aadria
                    feataa* aad aaryaaaa-a^t  baaaUaa ••oaratioa of
                                      •UC; baaallaa aoaaracloa of aadria
                                          jf  aaicM of ettrysaao i^c
                    >40% of •ochaayiimor paak aaloa*.

         9.2.5.3.2  tt* aoaaitlritr — Sloaal/aolaa ratio of >S  for a/s
                    241 of atey»aa«-d«2.
         9.2.5.3.3  M oallbratloa —  Abvadaaco of a/s 241
                    t» taa« of a/s 240 pvocacod by Garr»«ao-*i2 U >1S%
                    aad 05%.
         9.2.5.3.4  tack of ilaygadaKiaa of •adrla.  fiwalao aa SXC9 far
                    a/« §7 la taa ro«aa«laa uaa wladav baevaaa 4,4'-oos
                    aad aadoamlfaa valfatat ooaflxs taam taa ataadaaca
                    •f-a/s «7 at taa rotaatloa Uaa of aadrla aldabyda
                    la <10% that of a/s «7 prndaaad by aadrla.
         9.2.5.3.5  Lack of docradatlaa of 13C.,-4,4'-OOT.  txaalao SICTa
                                             •12
                    fa* a/s 291 aad a/s 247 la taa rataatloa tlaa window
                    taat lacladaa 4,4'-ooo, 4.4'-OCE,  aad 4,4'-oOT: a/s
                    2M w««ld ba prodacad by  3C13-4,4'-oo«, aad a/s 247
                    by  aC15-4,4'-OOO.  Canfira tttat taa total abuadaaca
                    of ba«a laaa U <5% of a/s 247 producad by 13CU~4,4'-QG>?.
                           C-15

-------
 9.2.« ftaalieaca  Aa*lr«aa  «< C*ta  —  U  all  parroauaaa encarla  &r«
       •aalyaa  on*  1- or 2-rU,  4liqoo« e£  «*c& o£  tha ochar  four
 9.2.7  Xaapaaaa  Factor C&leol*eloa

       9.2.7.1 Calcalaca  fftva raapaaaa faceara  (W»)  far «aeh paaclcida
              •aalyva, Ka califeraeloa eaaaaaar, *ad sarroqaca coapouad
                                    (Saa Saca.  12.3.2), saaaaaciur«aa-d10  «ad
                          •  iataaxaca* iaa «toonaaaca a< qoaattsaeloa
                             iaa far a paacieioa. * yea
                             coa^aaar ar a lonra^aca cc
                             ta*«»r»«a* toa atowaaaaa at a/« 240,
                             aa «aa iacaraal scaaaara «g a/s il«. «ha
                             faaavitaeiaa iaa wfeaa paaaaacAraaa*410
                             la aaaa aa tfca lacanal ««aa4ar«,
                                                               or
                             aaUbraciam aeaaaaar or rarra^aea eaaaauad.
                 la a ooitlaaa aaatoar« mLta oaa4 ca
                   aa a^olvalaaa.  Ha«at  THa dj-PGI eallaraeiaa eaaaanar
                      ba raaal^M teas alaaa-UC.  £2 aa«, alyha-IK will
                   i*«ta ta cfta iaa aAoadaaaa aaaaoraa far C12-K3.  79
                    "  far dtu eaa«rtba«ioa, «oftcra«« «.r% g< e^a iaa
                        o< a/x 219 aaaaora* for 4ipha-WK fraa Ua iaa
                    aaa aaaaora* far a/i 222 far
9.2.«  Raaamaa Faetar Xapradwaiailicy —  Far aaafc paaxlclaa caalrea. 7C3
                   caaaaaar «ad surraaaaa eaaaaaad. ealaalaca cha aaaa W
                             at taa fivo OOJ.  MM* tha RJD aMaada 20%,
                                            rlaca OU ca obtain
                       taa aa«lra eaaaaatra«loa raa^a. ar caJca ««ciaa ca


9.2.9
       9.1.9.1  Yd aa«aaiaa«iaaa - Atoala«a racaavlaa elaaa ot »C1 eaa^aaars
                •77 *a* «1Q4 shoaltf na« vary by aara CAaa «10 • frea oaa
                aaalyala ca caa a«c«.  (ftacamiaa tlaa raarodnelbilisr  i*
                aa« «a arltical for eaaaaaara »t tad »209 aa for «?7 and
                • 104, «4Heft 4ra oaad ta oacacalaa wtiaa ton sa«a «r« eftanoad.)
       9.2.9.2  faa«ieioa daxatainattona — Aaaaloto ra«aa«lon claaa a<
                         ordaaa, cadoaulfaa I. ana andaaulTaa ZZ shaald  ne«
                     by aara c&aa ^10 • fzoa oaa «aalyala ea CJta nan.
                              C-16

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  9.2.10  to cord a spaoanB of MCS CAL
9.3.1  Witfc tha following proeaduraa. *«ri£y initial calibration •« tha
       hoftnnlaa- aad aad of each 12-a pariod during wfeich aaalyaaa «ra to
       ba paxfocBad.
9.3.3  Calibrate tat ewa tho Hi with acaadarda and prooadaraa praoeribod
       by tfca
9.3.3  JUMirM * 1-«L or 2-vL aUqv« o< ttM OTT»» M
                  Hi eaUteaUaa aad parforaanra (Taftia 4).
9*3.4  Ia3««« a i-«& or 2-«L allqvM «rf tfta Hadioa Oft and aaalyn
       «aa« cvadl&loaa oa«d 4wia* Xaitial CaiUratioa.
9.3.3  Oaovaatraca accvpeaala parfosaatwa far erttarta daaartbad la S«ce.
       9.2.4.

9.3.4  OacaaOM ftha* aalthar tte araa Mamrad for a/a 240 (or ctoyaaa*-^!2
           ttoaa Car a/» lit far phanaatrtrana-4^Q haa dacroaaad by aora cbaa 30%
                     aaaavad U tha aaa* racaavarrvtooa aaalyala o< a
                   aalaaiom ar by aara taaa 50% froa tha aaaa araa
              ialtial ealU»ra«Xaa.
9.3.7  Raapaaaa factor teyrodaelbilley. —  for aa aeeap«atoLa Cantlatiin^ Cali-
       bratioa dock* tha aaaavrad IV for aactt aaaZy^a/aurro^afta eoapouad
       aaa« ba wtchla *JO% •< tha aaaa ralua ealcola«ad (S«ee.  9.2.7)
              laittlai CaUttracioa.  IS aoc, raaadAal ae&toa ana« b« eakaa;
                     aay ba aa«aaaary>
9.3.1  S2X taaiyma Ma«aatOoa ttaa HaarodualhllXcy — 0«aaaa«raca aad
                M*ap«ahla (Sa«a. 9.2.9)  raaro4a«l«Uley at abaola«a r«««attae
             of aypropriaca paaUcida «aaiy«aa aad Kl racaa«loa tiao eoa^anaes.
9.3.9  faaadlal aotioaa aoa« ba takaa U eritarla ara aa« aa«;  poaaihla
              i arai
       9.3.9.1   OMOk aad adjuat « aad/or « oaaracia« ceadlciona

       9.3.9.2   daaa or roplaca iajactar Uaar.

       9.3.9.3   Flaah ooliaai «l«h aolvvatt aa«ordla« to
       9.3.9.4   Braak off a ataon portXom (awroAaataly 0.33 a)  af tho
                      ii  e&acJi oalaaai parfooaaoa by aaaiyoia of parfo
       9.3.9.5   MofUoa QC eolaavt  parfoaaaca of all Initial calibration
                            than raojolrad.
       9.3.9.4   A4]ua« MS far Creator or laaaar raaolation.

       9.3.9.7   Calibrata rtf aaaa Mala.


                              C-17

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            9.3.9.9   Yraaara and aoalyxa naw concentration calibration/
                      aarracaaaca c&acfc aalatiaa.

            9.3.9.9   Vrapara now concentration calibration corrals).
10.1  uaoMfOxr uftonrr suuoe out  — Mrfam all s«aaa ia th« analytical
                (Saaclaa 11)  ualaa; all raa«aa«a, •caadarda,  rarraqaca ccaaooada,
            w«« aaaaraeaa*  flAaawara, aad aalvaaaa taa«. would b« oaad Car »
             aaalyais)  ba* oait «a allqaae at saaaOa (waca» o* aail/«adlaaa«).
                 aaalaa, saAavitBCa 1 L aC raaaaac «««ac.  Z
                 P»-pru»ldad raaaaa« blaaft aaild aa«arl*l far aa
      10.1.1  ia CU ana* caat&ia tii« •«•• taeuaft of sorraaaca eaapooada «nd
              la«ac9Al ctaadarda eiuc i« addad ca aacH •••ala.  SUJ aaoua-e
              vtll *»rr wl&A *aaala «rpa aad wtea caa eypa of da«a
                          or SIM).
      10.1.2  Aaalysa aa Uta bafara aay savalaa ««• «rtraec*d aad anal7«ad.

      10.1.3  Sataca * aav bates of aai*aa«a a* r«««aa«a U oaad Car ««aaL«
              av«xaa«laa a* tor aaiiaam dtrraMtnyrayhtft araaaduraa* aaal/«a
              aa UB.  Sa addltxaa, aaalym * Ufeantarr aalvaa« bUak (U») ,
                    la ttta MBM aa aa CU avaay* eftac aa «arraaa«a eaaaevada or
                          adwda ara aadadi thia i1aaaa«trn»a taat raa^antts
              caacaia aa taaaa«lt*«ioa iaaa Car taaaa
      10.1.4  Aaalr«a aa Uta aloa^ wtcA «ae* batch of ^20
      10.1.3  Aa aocaauMIa U9 contitna aa aa«had aaalrea a« a «aa«aa«ra«laa
              araaca* eaaa aaa half of ita MOC aad ronritni M addl«taaal oomaauads
              wtttt «Aa«taa cJura«Barl««laa aad aaaa jpacigal Saaeoraa sAae would
              IscacSara «is& Uaaxl^lcacxaa aad aaaavr«aaa« of a aa«ted *aaiyt«
              a« l«a m*  £S taa Utt BB«« waa «a«raecad alana; wiea a baeeft of
                      La roair aal nairad  Kba «a«Xra bacen of •••al««
                      tad aad raaa*lr****
      10.1.4  earvaa«lf« avtlaa. far «Maaa9«aala Utt — da«k aa
                        aad fl«aaMara ea laaaca aad altaiaa«a taa aougea of
                            bafara aay laaaUa ara a«txa««ad aad aa«lr«ad.
10.2  GttXBMSZai — laaladad aaant ^nf*^1 aad namlnalm oallbraciaa proc«dur««
                                 eallarattiam aftacfea ara aaaaByiiaaad with  raaule«
                       «aa aalsciam, tfta aadlia* Laval e*llbr««iom aaiutlaa ear
                 laca tf«a of data aeajouxtiaa. aittar fuil-ranaa ar
      10.2.1  X£ MB* orltarla ara net aa«  ear a eaaclaolaa; C*ilir»eioa Chock
              a£ta* * 12-ta pariod 
-------
       10.2.2  Vhaa aeaa* eritarla la Sa«t.  9.2  ara not, M«,  mult* for affactad
               aaalyeaa ana*  b«  Labalad aa raapaet to alart tha  data aaar of  taa
               obaarrad problaa.   Zaelodad aaaaa; theaa eritarla  am raapeaaa
               factor  eaaex for  «ach  aaalyta ar  fa ealltoratloa  coaaaaar,  daara-
               da«10a  of DOT  and aadxla,  and vataatloa tiaa rapradueiblller
               SZM  data iiiyil iirina.

 10.3   UUIULE,  LiVIUHnUffZO*  OT  UWMSO0 CJtfMZLZTT fO* iam  MOLTSB
       (Xaavfflelaa* laftraatlaa la ewr«a«lr av*xla»la far liannamn in  far
       •all/
       10.2.1  Oa«il  apavoarlaca Qoailer Caatral OMek Saaplaa ar«  aralla01a.
              •aatt LiDoracary stwold prcpara aaa ar aara  aalaclaaa eaacalala^
              aa«a aatted aaalyca  at a coa«aatratiea eectaaBundtay «o  that  aatlel-
              pa«ad  la saaalaa.  Oatil a«eva«y aad praclalaa llalta iuva b««a
              aatabU«aad far »C1  laaaar froaaa la asfraprlaca  laaplaa, a aalotlea
                         aa Axoclar alxaora aay »• oaadf  eaaaara total aaaatsrad
                         ratlaa oa taa tatal Are«ler eoacaatratlaa.  Xapore
                           ttratlaa aad aaaaorad eaacaavraelaaa «£  K3 tioaar
                         total aaacorad td «aa«aa«ratlaa.
      10.2.2  Add aa cperaavlata valaaa a< a *ala«laa «t aattiad aaalytaa
              «• •••* •< Sao* l-C, all«^a«a af raa«aa« «atar.  firtravt aad
              aaalr«a acoardiaa; ta avacadaraa ia Sa««. 11.
      10.2.2  for aaaft aaalrta, ealcalata aaaaorad eeaeaatratlaaa, ralatlra
              •caadard da^latlaa of taa four aaaauraanta, aad aatAed hiaa
                     12.4).
10.4  UUOIUSOXT fntPBMAItCX CUQC SOL3VIOV — Za "M - aathad* tha naitlna it
      aeaaaatratloa aallaraclaa aalmloa alaa aar^va tha porpaaa a< a Uboratary
      aatfaauaea attack aalatloa.

10.5

                                         rf bach iimuaata eoBpavada la
                                      aeeaptaaaa Ualta hara baaa aataaUahad far
                                   tte fallowla* aaidallaaa ara providadt
                                 CM • -JW «• *10%» aaaaorad biaa with
                                             • -40* ta «2S«.
10.4  QOfcZTT OWIMi. vjgfl saionx — Ham ra« amllaalai aacletaaca aa«d far
                                      f ^20 laaajlia.  It fullTaaav data ara
                                       aaaly«aa «aa ba avcaralaad wlta aaa
                                           »M amraa«laa aad o*« OC/1VJ aaalyaaa
                                            aad paatloldaa.
10.7  LMOU9OKT SVO3D OOftSASS UMfLS — S«la«c aaa iaaplt from aacb batch a<
      i'fl iaaplia at •lallar trpa aad fartlTr (*•!*•> tM allo^ou a< taat saael«
      »lta a Mloclan eeatalalaf «pproprlata eaac«atratloaa e< paatlalda aaalytaa
      aad at Uaat aaa Aroclar alxtva.  AT tar addltlaa at ««rroaata eoapeuada,
      ajreraot aad analrta (S««t. 11) taaM tw« farU^lad all^at* aloaa; with
      aa addttlanal uafartlflad saaaOa alJ^aot.  HaUtlTa dlffaranea (W) aC
      duplleata ramle« tor nrraaata cnapaniid eMMaatratlana «tto«ld ba <4Q\.

                                    C-19

-------
          (» • [C, - C2 / 0.3 (C, * Cj)l  100 )   Calcalata biaa aat la a 230-«b trlaaaarar Sliatt.  Add * *aeaad
                            «»Iavi of aatitfloaa e&Larlda ea tfta ••••X« bo«tla «ad
                            rapaa« e&a ••craotioa acaaaduM « taeaad
                            efta anxmeca la taa ttlaaaaya* £laak.  >«rfatm 4
                                       la t&a *aai
                                                       (X-O) eaaaaacxatav by
                  11.1.1.4  Vaav taa nartlnad axtraam la«a 4 aal
                                                    10 OB o
                                                       «ita 4 20 ta 30 ad oartxaa of
                                      ealavlaa. 4ad 4dd tfca rlaaa ta taa drrlaf caluan.
                  11.1.1.S  Add oaa •» CM eiaaa balO^av olUaa ta taa
                            Claak 4»d 4ttaA 4 tftr«a»aall Sard** eaLuam.
                            taa Sayoax ealiua* by 4ddlaa; 4aawt  1 at of aacftylmo
                            ealotlda ta efta eoa.  rlaaa taa K-O 4aoaratau  on 4 hat
                            M«a» ba«a (aO-«S*C) aa ttta* tfta ceneaa«r«tar  tua« I*
                            partially laavraad la tha hat ««ta*» 4ad tha «ntlra
                            IOIMV rovdad awrfaaa of taa Claak U batftad wlt& not
                            T«aar.  Adjoat tfta vanOeal poaltlon of  tAa 4aaax4tna

                                        C-20

-------
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                               BS*T«tfB«Mv —
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                             »*a»np««* "JB-OOOI • Ba
                                qa aa B7»aoq rrd»w
                             T»«T*T»B B^a BrfvzBaBo  ft
aT BBV >r»rr3 Bqa
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                                             a JCTT
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                     01 »B»»I a* ae; TBB» BB*
                   a«a»*» Bqa Boa? namndo* o-l
                        ft> BVHTBA »B«2«dd» Btja BBBJI
     BB«BBpBB»
    B»BJ aBdoad B^a av  *«TB ot-6l
           ea

-------
11.3 CC/M
    11.3.1    taawre the sample extract or blank froa storage and allow it to
                    eae laboratory temperature 12 oeceaaary.  with a stream of
                  filtered aitroeea, reduce the extract /blank volume to the
             appropriate volume,  depeadiaa; «» aaticipeted aaalyta concentrations.
                 aa appropriate volume at the •yprapviaea ia««rmal «taad»nl stock
            11.3.1.1  Xatunul scudacd eaMwitrmtioa far f«ll-ffaaa«
            11.3.1.2  Zatanal »taad«rd eeao«a«ra«iaa Car SIM data
                                  • Q.79 a^/at «<
   11.3.2    Iaj««« 4 1<-q& «r 2-«C. «Uaj«0« a< taa aiaak/saaala extract lata the SC
                     mder caadltlaaa tued ta pradoce acevvtaale reaulta 4uria«
   11.3.3    teejoire aa«a •aeecral data vita eltaer («U«raae« data teajolsitlaa
            •aaditlaaa a* SIM oeadlUene, «• aperaenate.  ?«e the •••• data
            •eojiaaltioa tlae aad Mi operatXaf caeeUtioiw pre*ie«aly ued to
            deteralae reepaaae It
   11.3.4   TirMlne data tor satsvated laaa ia «a«a ifectra 
            if satorat^ea oeevred. dXlate aad reaaalyse the extract after the
            «joaa«lrr a< the tataraal itaadarde U *dju«ted aosraerlately.
   11.3.3    Foe eacft laterual rtaadar*. determlae that the area aeaaqced ta the
                   evtraet hae aom ieereaeed by >30% froa the area aeaaured
                   the aevt reeeat arevtooa aaalyelj a* a cali&ratlaa •oitttlaa
            er *f >SO% Sroa the aeaa area aeamred dorlAf Initial «aiibratian.
            If either ezltariaa L» aot aat, reewdlal actlaa eoat be takea ta
            iaprore seaaitiTtty, aad the saaaie extract aaat be reaoaiyted.
                   nta
    11.4.1   Oaiae; the iaae ia»*« la Tafelea ?a*7« far Vda ar Taste 9 Sat
                                            pre
-------
        11.4.2.2  Obtaia  iataaratad abwdaaea areaa  for qjuaaeltatlon aad
                         fttiaa ieaa.
 11.4.3  SZM Data — Obtain  appropriate  selected ioa eorraat profile* (SIC7»)
        far ZS qoaatltaeiaa «ad eaafiraatlaa  ioaa,  for  eaea Ion aaaiterod
        «o data** peetieidee  aad  ete  surroaata  compound*  (Table 9),  and for
        taa *jaaatlta«loa aad  caorlasatloa  iaaa  far  e«ca KB i*oaar ?roup.
 11.4.4  Kl Aaalytoa

      11.4.4.1  for «il KB aaadldataa. eoafixa tha proaaaca of  aa («-70)*
                iaa olaatar by ewaortnlae;  XC9* or «pactra  for *«  IM*« on* of
                taa aaa«  iataaaa  laaa  la  taa cyeraarlaea  iaa eiu«ar.
      11.4.4.2  for Clt^Cl? iseaar oroapo,  ewoaina  XC3>* or  spectra  for
                aaa)la, i«4% af tha aroa aaaavrad  for  a/s  322 should
                ba Bttbtraatad froa tha area aaaaorod for a/s 324, and 10«% of
                taa a/s 322 araa shamld ba  sobtraerted froa  tha  aroa aaaaurod
                far a/s 32« (Tabla 13).

                                                     IO« or spacers for
                        (*»1SJ* iaaa that <»ejalit iadleata a  eoalatXae; fd
                               additioaal a&larlaa.  Tax* eaalatXan cause*
                              laaaaaa of **^ aatoral abBadaaoa  of ^ ^C.
                CSt&» iatarfaroaaa will ba  ssMll aad eaa ba aafl*«tad except


                        .) Ta oarreaa far thX* iacarforaaaa, obtaXa aad
                       tha araa far taa appauaalata lorn (Table  14)
                    (!*»D* iaa  data ta oalcoOata tha ratio of  tha  aaaaured
        peaii aroaa of tha qoaatltatlaa iaa  aad eanflaMtiaa iaa(s),  and
        ooBparo ta tha acceptable ratio (Tabla 9 for paatXeldaa and Table 12
        far fda).  IS aceeptabl* ratioa aro oat obtainad.  a eaalatXne; or
        partially coaltssiaa; ooapoqad aay ba iatarf erinc.  Zxaaiaatioa of  data
        from sawaral scan* aay prorida infonaatioa  that will allow  application
        of aAdltioaal baekeroqad correction* ta iaarowa tha ion ratio.

                              C-23

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11.5* zJJUMxrxc&rxoM exxszita

      11.3.1  Xacanal Stiadarda
            11.3.1.1  CJsrr««B«-<412 — ftna •buadaaca at a/s 241 r«La«iT« to a/x
                      240 aaa« ba ,>13% «ad <2S%, aad c&aaa ton* aua« aaxlalxa
                      •lault >aaan aXy.  tha axaa aaaavrad Sor a/x 240 BO*C ba
                      vitala 30% atf eaa •»•• aaaawad dorlav ta« aoa« racaae
                      ealiaracioa.
            11.5.1.2  »«a*a«ar«a«~41 0 — to* «buad*a«« otf a/i 10» ralACi-r*  to a/s
                               b« £10% aa* O2%, «ad «&••• lea* «u« aayiai »•
                                       Th« «ra« a««««v«d for a/i  it« aore b«
                             30%. at tH« «*•« aa*«w«4 dovta^ ea«  aeve rveaae
            11.3.1.3
     11.S.2  IMU«IUa4« teca Jar »w«laida Aaalyu* *«* Sum****
            11.5.2.1  M«aa«l«a ciaa a* ta« ••••!• ««Bpaa«a« atwc a« wtsaia  «  *
                      atf tJM claa ota«xv«4 to* «aa« •«•• auapaiutil «ti
                               waa «aalr*a«.  Caieola«a ctta valua o<
                              . « • (le)1/^, «Har« IS • oba«rv«4 rvcaaclaa
                      (la Meoaaa) a
            11.5.2.2  All iaac vteft raiaciw atooidaaea >10% iA «ba aaaa
                                    « la caa aaaa sp«««raa a< caa eaadldtea  s«a«i«
                                 * wlamlac laa wlea ralavlf* «aqadaaea  >2* in
                                        na aaa« ba ?r«a«a« la cha «aadlda«a
            11.5.2.3  •»• laa «aa« ««a t&a aaa« «boadaa«  (baaa paak)  la «ft
                                         a* «aa baaa ?««k la «aa eaadlaa«a
            11.5.2.4  ra* Ul laaa with ralatlra ttMadaaaa  >20%  la  tfta  scaadard
                      •a««*nB, efta raUclva  ifttiailiaaa  la caa eaadlda«« •?•««•
                      aaaa a*a *a*y by aara saaa «13% la pareaaeaa* \«X«a (!•••,
                      U 10% la ««aada*«. max ba'%35%  tad,  <«S%).
            11.5.X.5  Zaaa wlta tatatlra  ifcaadaaa-a  >10%  la taa aaadlda«a

                                    Car by  «aa  «aalr*««   *«• '*•«* 7recaaau»9
                                  «a«4 «• abaala  oaadldaua •faotra, boca pcoeaaaa^
                                                    ba avaloacaa.
     11.5.3  S3X Oaca  »aa*loida Aaalyaaa  aad. l«m^a«a C
            11.5.3.1  XbaalBta  rvtaaelaa tla* a<  aac* mrraaata eaapeuad &ad
                      paaxlolda eaadXdaca aaa« ba wttiiia 10 • at tfta«
                             tfca  La«« pravlaua «ce«eubla
            11.5.3.2  All laaa  aaaltara* far aacft eiay	d (Tabla 9) auac ba
                      praaaa* «ad  aoa* aa«laX
-------
               U.S. 3. 3  tn « apacem tvaraqad acroaa • « paifc tad with  baek^rooad
                        carracbloa, 12 aaeaaaacy, tha aaae 4&uaduc ion auae
                        wttft «abla * data.

               11.5.3.4  Oaaarrad ralaeiva •boadaacaa of eaa ae&lcarad  ioaa suac
                        aaac taa fallawlaa; critariat

                          VLdrta — a/* 2«3 • >20% cad a/s 2«3 •  >13%
                          |9C (3* «ad m/a
                                     X «ad IX — «/s 339 • >3M aad a/x  341 •  >20%
                                     mLe»M — •/* 274 • 40-99%
                                 — •/« 2«3 • ^30%
                                 •Iteiird* — •/« 34S • >10%
                                 IM-COM — •/« 317 • _>3»%
                                     — •/! 271 • >30? «atf a/s 274 •
                                     •paalAa — a/s 3S3 • >4fl%
                                   Lor — a/s 221 •  3-30%
                          rrarrtitnr — a/s 407 • 43-93%
      11.5.4  roll-taa^* «ad sm Oa«a far
                        wltaAa £10 • a* taae aaaaorad 4urla« taa L*a« jrrrioua
             11.5.4.2   fl«aa«lta«laa «ad eaam la Tmala 121 •« laaa« oaa laa la eaa  (»-7Q)
                                         ba
12.  CatOTULTIUM
    12.1  PTW apf>epclata XO« a< qoaatlutlaa laaa, «baala «ad raaard Ua  apace
          saaaaa' otf caa ajvaaaaaffaajaXa paak tpaai aad taa traa 9t sh^ aadxa
                   raphla paak.
    12.2  For Vda.  s«a taa araaa tor all Uaaan Idaaeiflad 4t aach  l«ral of
          ealarlaaeiaa (a.f., *oa all ^oaavltatiaa laa traaa Car Cl4*Vda).
    12.3  CalcoUtta taa caaeaatra«laa of ••« •tsr*a^a«a eupumid, paaclelda
          eaadidata. «ad Kl laaaa* iroap oalaf tha
                                      C-25

-------
           »ara  Cg  •  eaacaatraeiaa (aieroor*** par fcilovriai or aicroaraaa
                        aar Utar) of lurreaaga eoBeaoad. iadirldual pavcleida
                        or * KB ijoaar oroap*

                 A,  •  taa ATM of taa ojoaaettatlaa iaa ter aaea paaticlda
                        Aaalyta/iua iuaata ccaioauad or taa ma of «juaa«ltaeiaa
                        1*» iraa* for Ul KS iaoBMra AC a particular Laval
                        of
                     •  tha ATM of th« laearaal •«aadard qoaaelta«loa tan,
                        a/s 240 far earjiaua 1^3 or •/* 1«« ear aaaaaa«hraaa-4iQ,
                                 (aierofTMM)  of latanal •cudard Addad ca
                        taa arcracc bafara QC/Ni
                 XT  •  ealeolacatf raapaaaa faeear far taa «urTO«aea eoapound,
                        taa aartlalda reaadard. or taa KB eaUara«laa compound
                        far taa liraiar arovy (!•*•! of eaiartaactoa), Aad
                               (lOlaaraaa) of »tm^» aMraeead.  ZS A Uajoid
                               «M onraccad. 9 tmraaaa T, t&a wli»a 
-------
   12.5  ftapan oalcala«*a valo**  ta  «••  significant fiov**
   12.4  MM* atBpl** of teoowa coapoaitioa  or  far&ifiod *«Bplo* ar*
         ealc&Ue* ta* pareaat aacte*  bia*  aaiaa tha oqaatioat
                     • - 100  (C,  -  C,)/
                           «r ataraaraB* par  Utar),

                                          ta  ta*
             •otat   a* ala* ralu*  roealaa a po*itiT* or oaaativ*


13. AffTOMXT8P SSPffl/IvIATSOM AMD HLVSU^PfRff
                                for attaaA«*4 tteaclfieaciaa aad
    fd« (I)  uA p««%iald««.   Ottyro«M<«d «C/W
            Mr MOB  pa««ici4«  ••*  MOB TC* !«••* 9*0*9 1* eai«aiae«d «tt
            OUb^ia«tau«l  for fwavr la^anacioa.
14.
    7a ote&ia tia^l*  lAAoratDty 4eearaey «a4 pr«el«laa dtta for aached 40*1-/tM,
    rapilemea 1-t «Jj^ooca  o< r«M*a« vaear «ad ri*«r «•«•«
    «awa«J of  *BAly«M  war* *HU»«I*A «a4 4aalr«*4.  tauaat*a aroe*dur«« «*
    «• itfaaclfy «a4 a*aa«r* a*tha< «M!T«MI la 2««L Allo^Ma of 1-«L
    ••**•*• • raffi«i*B« o^aacier of iativlrfaai KM caaf*a*cs Ma* oac
    Ar««l*r aixtw**  war* oa*4 «• fartl^r «•«** ••plo*.  T&i« U ao« o**iraal*,
    ta«*a«* iatflTltaal VCB* ia Aro«Lors vary la oMcaatxscloa.  A* Aroolor eaaewt-

    will Call talow ta*  «*«**cl*a Ualt «*4 will a*« ta M**ytfi*a
    Za *adl«iaa, iA*offiot*a« daca ar* •«mll*01« «J**t Aroclar ggapaattloa ta «*••*•
    **eara«r «< iaoa*» *r*ap aa**a**a*ac* or t* •*•*•• MDU far VC1* «d*a Axoclors
    •r* «••« ta fortify  •«
    14. 1  ••*!»• t^wl  a****a« v««ar fictratfca — ri-w «U^a*«* of r**o*a« va
                  vita «•*•  latflTtdaal »**«Mi«* •« 4 o*a**a«ca«loa of 10 «*/L aad
                  1231.  1242,  12*4, aa* 12M 4« n*a«aamUua* of S «•/&, 90 «*/L,
         $• «*/L  4*4 2S
           4* of *2^ far 411 21 »*«ci«ia**  (T4»i«  IS),  far iaainteal p**«xeld**,

              f*r  *ateia 4loaBy«a.  «•  «ra* vala** 4r* laaum far eaaeaatratlon* of

        va*  110 a*/b  (UD 2.9%), «aiea iaaiaa«*4  4 **tta4 bla* of *13%.  for
        la4iTlteal Heaar «roap*, MO* of a*aa *aa*w*a eaacaatxaeloa* raaovd
        fraa 3.*% ta  16%.
    14.2 Low trral  x****at v*tar  fictzaet — N****a« vatar «** far«l£i*a with  «*ca
        po*tlelda  *t  «  eone*atr«eiaa of 3 «•/!• «a4 « tatal PC3 eoacontraclon of
        27  4«/L  (&ra*lacf  1221,  1 ao/Li 1242,  10 «*/lj  1254, 10 uo/T,; aa4  12«0,


                                     C-27

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                   Waaa aavaa roalicata cxtracta *wra aaalyvad^  aatbad biaa for
         iadividoal oaatieidaa raaoad from -17% ta *20% vita a aaaa aathod hiaa of
         -2% (Taala 13).   Aa MCZ, vaa caleolatad for aaca paatieida uaiao; tao oquatioa
         r«latiao: tao standard deviation of tho sawa roolicaea  aaaauraaoat aad
         seodeat's JB mloa tor a oao-tailad taac ae tao 99% eaafidaaea lovol vitft a-t
         doonoa of~froodoB d).  Wita tfti* calcalatiea. not, la  dafiaod aa


                           tod la wraaliaciaally low Wta raao^av froa 0.2 to
              tor paattLaiaa aaaly«oa (Taala 13).  A KB «, ia aa ladiridoal
            raoeariatic aad oaaaoc aa dotaxviaod victi saBalaa for%i£lod witb Ajredor
              roa.  CatiawftM of HOta far iadirldaal eaapaamea  of KB iaoawr oroopa
                                            tacal o^uacity aaaatvod for ««ch Uoawr

         iadiTideal KBa alao woro «ar«ali*xicallr low (0.01-4.1 io/t,> bocaoao of
         cao oacalloatt prooiaiaa of aaaaoroaaaea.  A aara ra«lia«ia ««a«aaaa« of
         da«octiaa Uaita tor paacioidoa aad KBa eaa bo favad ia Soct. 1.2.

   14.3   Xirar vaear txeraesa — n** allo^aaca of riv«r *a«or foreifiod vita
          •aaa paa«icida a* a eeaeaacraeioa of S uo/L aad total  KB eoaeaaesatioa
          of 70 tt«/t. (Aroalora 1221, 2 «o/Li 12«, 30 ao/bi 1254, 30 a«/Li aad
          1244* 4 »o/t) ««ra «Ara««ad aad aaalr*od.  Mo«Ba4 biaa for iadivtdual
          aaaxieidaa raafad firoa -30% ta «4% wteh a aaaa of -4%  (Taalo 13).  no
          oaeallaat proeiaioa of aoaaorod p««tiaido KB iaaaar croup eeaeantratioaa
          «aa iadleatod by MOa raa^la^ toaa 1.4% ta 7.3%.  •»•  aaaa aaaaurod total
              eeaeaaaratioa of 31 a«/L (TOO 2.3%) indicated a aattad biaa of -27%.
13.
     1*  Aaaar. J. A., 0. t. r»an«, 0). 0. NcKao, 4. A. Qoava, aad *. &. tadda,


     2.  lalUoaaitar, S. aad N. Sail, froaoalaa Z. Aaal. O«««, 302, 20, 19*0.

     3.  *Careiaooaaa — T*or*ia^ wiea Ca*«iaa«aaa* • Ooaartawa* of Boalfia S«rrtca,
    •Careiaooaaa — Mrxiav wiea ca*«iaa«aaa-, ooaarsaaav ox aaa^sa
    Caatar tor Oiaoaao CaacTOl. national Xaatxeaca for Occupational
    aad faalta, *«alieatioa no. 77-204, Aa^ta*. 1977.

4.  *Q4A Safo«r aad loalta Staadarda. G«n«ral Zadaatxy*. 29 CTK  1910,
    Oaoojaatioaal Safaey aad laalca AAvlaiatracioa, 04A 2204, *••
    *_^>^_ ««9A.
     S.  "Safo«r la HidaaH Oavlatay taa«ravrioa*,   Haartttin Otoaieal  So«iocy
                                         sal Safoty, 3rd Kditioa,  1979.
     4.  «lUa, H. 0.» C. TaaJifnf, S. Hamad!a. N.  MaaJaia.  S. I.  Safa,  aad
         U *. Safa, nuan Haoolotion KB Aaalyaiat   Syavaaaia aad  CtfomtaoraaHXe
                    of All 209 KB Caaaaaara*, ta^troa.  tci.  Tachaol.  14, 444,  1944.
     7.  fi«baarK, J. X*, ftayoo, T. t., Alfard-4tawaa,  A.  t>.,  aad v.  t.  todda.
                                            of                         .
                Grottaa*, Anal. Clam.  57,  2434,  1943.
                                       C-28

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<»T» i nov p«* 3.0*1
         OC
                          »*
                                                  R
                                                     *•;
       •a*oic
                     3.01 TO
•CM a 09
                                                              n«p
                     EfO X • OC
                                                                  f '•MV   *t

-------
     Taala 2.  Yd Caa^aaaxa 3««d »« Calliraeioa
                                            Chlorin*
  Kl tjeaar Croup       Mnaftir*          Sobaelttstioa
Caaaaacvaeiaa Cali&rmciaa Staaaaxa

  NeaoaaloraBlpaaarl         t         2

  Otealamatphaayl           S         2,3

                            29         2.4.3

                            SO         2.2',4.«

  feataehlorebiphaayi       «7         2,2* ,3. 4,9*

                           134         2,2' ,4,4', 3. «•

                           tM         2,2t,3,4' ,3,«,
  0«eMBl«roaLp)Meyl       200        2. 2' ,3. 2'. 4,5' ,4. •
                           209        2,2' ,3,3',4,4' ,3,3' ,«,«'
toeaatiaa Tiaa CAliiwtiaa

  Tncaealanbipaaayl       Tt        3, 3 ',4, 4*

  MatactaoroatphaayL      104        2,2<.4,«.<>

                                      2.J' ,3,3' ,4,3,5'
                     ta c&a *r*«aa «* l*U»«haAB«r aa4 Zall (2).

                                                         far be«h saoa-
                                    C-30

-------
                                                                                              8    3    3     3     .     „    -
                                                                                              sssrssSss
                                                                                              pppnppppp
                                                                                             -•*>«*«»»•*»*.»
O
 I
                                                                                    •^        ^™    ^»     ^»    w^     ^^    w*     ^»



                                                                                   I       1     I    1    1    I}    I
Vrapa
fee
Oil.
                                                                                                                                                                                     Z
                                                                                                                                                                                     s
                                                                                                                                                                                     *
e
D
&

a
                                                                                                    K-.     ^    ^     _•    _.
                                                                                                    MUOOOMUiUi
                                                                                             ooooooooo

-------
 ii
I  1
ii
 3
 3
 a

!j
 2  5
for
§1
                      sssssgsgsssssssss
           oooopoooo
           *-*-*-r«Mr«r«rtvi
                     ooooopoo
             e o
     j 333333533
            o e
                         M
                          ..•] «
                          M 6
                         999
       5
JB e r M • q *
3ll|3« ^f
jifsro 1}
        £i
»ii
         hi
                                             U II
                                                       CM

-------
Taala 3a.  Hmynaluiun asd Appraxiaaca Coaeaatracioaa a< C*litea«iaa Solacieaa
           tor SXX Oaca >c
-------
TU»la 9**  C(•pnaiu.ua «ad Approxiaarca Coac*a«rae4.oaa of CaJjL£ra«loa 3olu«loaa
Caacaa'craclaa ( n «/ot )
Aaalyea/Ia«araal Std/
Swroaaca Csapooad
U<*rta
BK, M« 1— r
4,4 '-000
4.4'-C«
4,4'-OOt
Oialdria
tade.«l£«i t
TnrtnanUaa «
BMoaoUu .«U»ta
ta*rta
tadna Utettyte
btfria Icatana
lapcaealar
•apcaealar apoaldai
HaHtaaMa1ar
s.a-1^ aaa* *__
Qvyaaaa^f]
FhaaaaaJg aaa- *i Q
^^-^-MC
13C12^,4'HJOr

cat i
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.4
0.4
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.73
0.73
0.2
0.2

at 2
1
1
1
1
1
1
1
2
2
1
1
1
1
1
1
1
1
0.73
0.73
1
1
C-34
at 3
2
2
2
2
2
2
2
4
4
2
2
-
2
2
2
2
2
0.73
0.73
2
2

at 4
3
9
9
9
9
9
9
10
to
3
3
3
9
9
9
9
9
0.73
0.73
9
9

at 9
10
10
10
10
10
10
10
20
20
10
10
10
10
10
10
10
10
0.73
0.73
' 10
10


-------
T»bl« 4.  Crltaria for ort»»
 127



 197
 199




 27S




 3U




 441




 442




 443
10*30%
            
-------
Tattia 7a.  Xoaa for Salaetad Ion Maoita*la«; to 0««arBia«
           Oa«a for Four *a«a of OS Xoaa
Vd Xaoaar Qroaa/
MaaaAlareaipaaayla
OieJOaraalahaarla
Tricfciarabiphaayla
•aatacalarablphaarla
laMchlarebtpaaayia
•aptaeblarablphaayU
OocaehiorottlahoarU
MaacftlaraUpaaayl*
OMactUaraatabaayl
«^,aa^12
"c.-~— -«:
13e.--4,4'-00T
N0** Wft«
1.0
222
294
290
324
390
392
424
440
494
240
100
294
344
Naaa or Maaa*
ta bo Noalearad
132i 104-190
220-224
294-240
2M-294
322-320
394-342
390-394
424-430
440-444
494-900
240-241
100-109
107,109
247) 249
na. of
Zoaa
4
3
7
7
7
7
7
7
7
3
2
2
2
2
Xoa 3«ca
•1 »a *3 *4
4
3
771*
7 7 1»
7 7
4« 7 7
44 7
7
7
3
2
2
                                                                29   27   24   33
at (M-7Q)* far d9<
at (H-7Q)* for
         •/« 294 ta m
     »*» a/s 210 «• iiiB
             «« •/> 397 la
             «« •/* 391  la Xaa
     100 »nd 109 iaclAdad 00119 Laaa «»** to 4a«
     107 «ad 109 laalaoM AMO^ lana uaod ta dac
                    •«aTva a
               ud aaaaora aanacAlorobiphcnylj,
                                   C-36

-------
                                                                    •ION
                                                                                           'low »««»1 "HO*-13
                                                                                            •tl-CI
M»
ICC
CC»'9C»'9C»
9«C't«t'CM  CC»'9C»'9C»'9C»
                                                     »«I'C«C'9«C
                                                CC»'9C»'9C»
                 99C'9SC'9$C       CC»'9C»
                     »CC'CCC   9«C'9«C'CCC
                     9«C'99C
                                                                                  9»C
                                                                                  9C»
                         "13

                         ••AJ
                         •13
                                                                                  99C
-
ccc
ccc
-
ccc
«9C
ssc
-
-
ccc
-
-
99C
»sc
-
9«C'9«C'»«C'CCC
C9C'99C
_
C9C'99C
9CC'9CC'»CC
»«C'C«C'9»C
-
-
9«C'9«C'»«t'CM
_
-
C9C'99C
9CC'9CC'»CC
9CC>CC'CCC
9«C*99C
9SC'»SC
C«C'9«C'«9C
9fC'9CC'»SC
CCC'9CC
991 '991
9«C'CCC
C9C *9SC
9CC'»CC
C9C'9«C
9CC'»CC
»«C'9«C
9SC
»«C
99C
9CC
99C
9Ct
C«C
9«C
                                                                                               'la
                                                                                                 6
MC
ICC
»«C'CCC'9CC
                       »cc'ccc
                     CCC'9CC
                     991 '991
»«C'C«C'9«C B99I'991'ttl'CCI
    9SC'9SC         qtSl'Cfl
                        SC«N
                                        •t«N
                                                         •l-H
                                                                           • 91
MC'9«C
    9CC
    »cc
    9«t
                                                                      ••Of
991
191
etc
9CC
CCC
991
                                                                                               ha
                                                                                                    'Cl
                                                                                                13
                      »*|J

-------
O
                                         a  «r

                                        MM
                                        O   O     «

                                        B   I   Jt*
    ?

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         »•  IT
         I  *

        ii

 I  I   I  i


 MM

J  /  *  i
O    I   I   I

 MM


     I   E
          •«
        /
        M
S   S     !
          a

          A

         *3
                                            A
                                                  I
                                                            .   if
                                                            »   lr
                                                                                                    a   F^
                                                                                                    *   *s
l£ ^J 4rf fc^ 14 ^^ 4J ^* ^4 ^* ^^ ^^ fe* 9^ fr4 ^^ ft4 9^ 0J

«4B«JkCtJO««l»«M
                                                                  A» LA LA 4^ bt CA ^4 t^A ^4 b4 t4 VA ^A bA ^j fc^ ^^ <
                                                                  fj3«««i<*3*4k«AMUMU»j3B*>
                                                                  Ha*»a^MS*^t»*»MOi§^
                                                          e-   o o <* «•
                                                          O   M O <• •

                                                          e
                                                           u   uu w u   if 8


                                                           » M O O » •     M
                                                                         u> A
                                                  i
                                                  ?
                                                                        cs

                                                                        n
•f     «I

*s     ;!
        «8

          J
                                                                                                                  S
                                                                         • it

-------
Table  t.  ftaeaaclaa
Oa«a for
•r <3r
                           •ad Calibration
       Sronp
MaaanhlnrnotoaaaTla
Oiahlaroalphaarla
TrioalarabiphaayI*
Taeraaaloraolpaaayla
Paatacaloroblpaaay la
laBacftlorohiphaayla
•apcacfelaraaisaaayla
Oocaehlaroaiphaaylj
naaaahlegealahaaylj
Oaeacbloreatphaayl
kpproxiaaca
Mtt Saaga*
0.30-4.33
0. M-4. 39
0.44-4.44
0.59-4.42
0.44-4.92
0.7S-1.1
o.n-1.2
9.99-1.21
1.14-1.24
1.3
Cal. Caaf.
1
S
»
SO
47
194
144
200
*
209
Cal. Cong
Mtt*
0.30
0.43
0.54
0.54
0.40
0.42
0.44
1.03
-
1.3
                                               a 30 • Z 0.31 am 13 tt-54 f
  »Uiea capillk*? ealaM aa4 ea« tolla«la« SC eaadltiamat spllslaaa
  *« 40«C; hold far 1 alAi haa« rapidly ea 140*C aa4 h«14 1 alar Laeraaaa *e
             310*C.
                                  C-39

-------
Tabla 9.  t«n« tor Salacead laa Noai«aria« Oaea Aeqoiaieioa Co* »«acleld«
          Xaftanal Seaadarda «ad 3 -------  --------- — '^-- ---- '  ^   -
ton
Aaalrca/taean
Surrovaca Cornea
Alpha-OK
o«ca-OK
«aa»OK
13C,~<*— -•":
»n.aaaea*aa^d10
Mea-OK
I«p«aealor
Xldrla
AL Std/
ad (MM
(2M)
(2M)
(200)
(294)
(100)
(200)
(370)
(302)
I«f«aaalar «paxlda(3*4)
liaaa rhlardaaa
todo.ul.-4fl :
JUaaa-ealordaaa
Tra»a-~acUa*
Dial drla
4,4'-0«
cao*ia
«a4amara.I2
4.4-«
MlatlfeArd.
(400)
(404)
(40«)
(440)
(370)
(310)
(37«)
(404)
(311)
(371)
taaoataUaa ml£ata(420)
4,4'-OQT
13Cia-4.4'-0«
Kadria kacaia*
C&r7Ma-4Y2
Na«Aoar«lor

(332)
(344)
(370)
(240)
(344)

Appro*.
0.43
0.47
a. 40
0.40
0.49
0.31
0.30
0.04
0.70
0.74
0.70
0.70
0.77
a. oo
a.oi
0.03
0.03
0.07
O.M
0.91
0.93
0.93
0.99
1.00
1.03
C-40
Qoaac.
ton
219
219
219
223
100
219
272
203
333
373
199
373
409
79
244
01
193
233
07
273
233
247
07
240
227

Zeaa (Apprexljuea
Xala^lT* Abundaaea)
111 (100), 103 (90), 219 (70)
101 (100), 103 (90), 219 (70)
101 (100), 103 (90), 219 (73)
1t7'(100), 109 (90) 223 (00), 227 (4
100 (100), 109 (13)
101 (100), 103 (90), 219 (70)
100 (100), 272 (00), 274 (40)
04 (100), 243 (40), 243 (23)
01 (100)., 333 (00), 333 (03)
373 (100), 373 (93)
199 (100), 339 (30), 341 (33)
373 (100), 379 (99)
409 (100), 407 (03)
79 (100), 243 (10), 100 (13)
244 (100), 24a (43)
01 (100), 243 (73)
199 (100), 339 (SO), 341 (33)
233 (100), 237 (43), 143 (03)
47 (100), 343 (30)
272 (100), 274 (00), 507 (30)
233 (100), 237 (03), 143 (43)
247 (100), 249 (43)
47 (100), 317 (30)
240 (100), 241 (20)
227 (100), 229 (13)


-------
Taala 10.  Zaa Sata tar Salacead Zaa NeaAttariaa: a* Paacietda Aaaly«aa.  tat«rn*i
                                             (Ordarad by Ra«aa«4.aa tlaa)
Zaa
                            Zam Sa«
                             H
                                                                 Meaiearad
                               •7

                              1«S

                              22?

                              221

                              US

                              237

                              240

                              241

                              247

                              249

                              271

                              274

                              317

                              34J

                              347
                                                                 4.4'-000
                                                                 tadaanlfan

                                                                 4,4'-OOT

                                                                 13C12-4,4'HSOT

                                                                 tadria kacaaa
                                                                 Mathoxyehlor
14 iaaa, •
13 laaa. 9 a
                                                       19 laaa    •  e
                                    C-41

-------
    1!
    a«
        N
        fL
    «oon*o»^m
    r» »- o ••»»•»- r»
n r* «i ft
1 « f- r» f»  •-« •
i »- r« o e  a o

       S"
                                              •- O t- W i
                                              • ^ f» O '
r» r> •- O • f»
*" H ^™ tO **"
                                   •* • •» o »• r»
                                   5 5 5 SS S
 8
 3
I
i
i
         O«9r*M*-«
         •»  o»-ll«-r»
J  «*
fro^n
• o •- n

f"
                          5
                          f

                          t
                              o «-*•-
               •3 o f?

                                               • t • •  •••«•
                                                                          01



                                                                          6
                                               35353733333555!
                                                 rt M
                                                 ^ *


                                              «RRR  pa««««sss«s  j

-------
Zatarnal Std.
                    tm
Coafiau
  Zoa
Tabla 12*  QoaaCitaeloa, Coafixaaelea , «ad Zatar£*raaca
           lacarnal *e*adaxda, aad
Qoaat.
 Zaa
                                                        OMCX Sou  for
XMiO*
  H-70  tat«rf«r«nc«
Caafifli. ea«c>c Ion*
  Zoa    it* 70  (t*39
         * Sroap
  Clj

  Clj
  Ci10
144
222
294
2*0
324
394
392
424
440
4*4
144
222
294
2*2
324
344
3*4
430
444
4*4
190
224
294
2*0
324
342
394
424
444
300
3.0
1.9
1.0
1.3
1.4
1.2
1.0
1.1
1.3
1.1
2.9*3.9
1.3-1.7
0.4-1.2
1.1-1.9
1.4-1.4
1.0-1.4
0.4-1.2
0.9-1.3
1.1-1.3
0.9-1.3
                                                                    192^  294   222

                                                                    192   292   294

                                                                    144   324   290

                                                                    220   340   324

                                                                    294   394   340

                                                                    244   430   394

                                                                    322   444   430

                                                                    394   494   444

                                                                    390    -    494

                                                                    424
244
144
2*4
344
244
144
147
247
241
14*
14*
249
9.1
4.4
1.0
1.9
4.3-9.9
4.0-7.2
0.4-1.2
1.3-1.7
                        l«a «a

                        laia Kl to
                                             «a  to« *« a/s 192.
                                   C-43

-------
tea Maaaarad % of tteaa. Zoa ATM to
cudidata Qoaot. Confirm, to Ootaralao b*» Subtracted from
Zaomar Croup Zoa Zoa Zatar£a*aaca
TrlcftloroblpboflTlJ 234 234 234
'leaacaloroelpaearU 340 342 334
loptaealorobiphearU 394 394 390
TabLa 14. Conaaxloa for ZatarCaraaca of KB Coatalai
Zoa Noaaort
Caadldata Qoaa«. to Oocarmu

TrIealoroalpaaarlJ 234 233
tatraeaioroatpBOBf la 292 249
•AMAtfteLA0Bk^A^^^RPtA 34A 3S^
•^•^^IVBftOT^H^PHW ^^M^^c ^" v^^v • w *
OcUMmlawaCAplMaRr^ 434 433
Qoaat Confirm*
Zoa Araa ton Vraa
99%
104%
141*
233%
>a« Oaa Additional ca
id % of Maaa. Zoa
M to bo Subtract!
ta STOB Qoaat. Zoa
13.3%
13.3%
17. 4%
23.0%
24.3%
30.9%
40.0%
33%
144%
71%
123%
lorlao
Araa
id
Araa

C-44

-------
•
w _
3 S

i I

to to
S J
S S
I 2
3
A
•
i
1 1

! *
« 3
to
> !
; t
t »

1 *

i i
\ M
i 1
r
t
n
•
i
j
5*
,
• >-
• 3 *

* :fl
:i:
13"
m
it
9

•
J*!
. ,a
il5
iji
K O 3

• «
« »-.
• a *
« . .
4 O ^m
»|*
IH


|!
«
i  t  » • i  i  i
    C-45

-------






tf
j
0
•

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g
•
3
4*
1
2
M-
3
s
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25
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3
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lit

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m
s:
2S-
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ih

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31

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1



M
M
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^"Ilt**1^"**

2 i i i i i i i i i i
i
1
fssssssass *

• UUUUUUUUUU i

72
i
t
T * 2
CC J
• « >•
to
2
• 9
• te •
2 5
" . 5 .
• to
J S
•• •
3 |

* •
T , . S
C a «
si
• 9 T to
2 i J" 3 *
- i i
Ml *f -2
• 1
M a «•
s : s
to M •
II M » M
1 ! «
it 2 • 1
« Q
2 ^
it ^ i. 5

1 i |
11 • • !
^ c • • **
• * >» >» 8
-2 : j j
» ] i • • «*
• 1 • MM*
f ?T- i i :
I 2 - 4 4 U
C-46

-------
    •ndoaulfan aultata
34. DOT
3S.
at.
37.
  . MthoMyohtor
3*. cita-rct
^
                II
                II
                II
                14. alpha cfcl*r«aM
                IS. tra»a-«o»aohlor
V*«ura I.  Tatal Ion Currant  froflla  o(  fcm Calibration Con«|an«ra and rnatlcida

-------
si
•t
II
i e
«*

II
I8
8
w
ll
I
.8
Li
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0-
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w
8

! :
          n
         M
            c
           s
             ?

-------